Investigational research on highly functional carbon and related materials (HF-CRMs); Tansokei kokino zairyo no chosa kenkyu

Energy Technology Data Exchange (ETDEWEB)

NONE

1998-03-01

The paper arranged a fiscal 1997 guiding study of highly functional carbon and related materials (HF-CRMs). In the material invention field, described were the composition by interatomic control technology and the characteristics of pure carbon nanotubes, carbynes, graphite, fullerene polymer, porous carbon, etc. Heteroelement substituted materials were also described. The paper also reported the application of HF-CRMs to the electric/chemical field, and arranged the basement technology and applicability of diamond in particular. The subjects are enhancement of composition technology and reduction of the price of processing technology. Especially, the control of impurities and defects is a must for the electric use. The application of HF-CRMs to the mechanical field was reported. Superlubricant, wear resistant and high temperature corrosion resistant materials were taken up, and were surveyed in terms of their use mostly to refuse incineration power generation boilers, and thermal power generation use turbines. In the development of mechanical materials, technologies were surveyed especially for large area/complex shape film formation to form films for various parts, functionally gradient film formation for relaxation of thermal stress and residual stress in the film, and high speed film formation for quantity production. 363 refs., 88 figs., 10 tabs.

Fresh biological reference materials. Use in inter laboratory studies and as CRMs

International Nuclear Information System (INIS)

De Boer, J.

1999-01-01

Biological reference materials were prepared and packed in tins and glass jars to be used in inter laboratory studies on chlorobiphenyls and organochlorine pesticides, and trace metals, respectively. The materials were homogenised, sterilised and packed as wet tissue, which is unique for the purpose of inter laboratory studies and offers the advantage of studying the extraction and destruction steps of the analytical methods. In addition to their use in inter laboratory studies, some materials have been prepared or are being prepared as certified reference material for chlorobiphenyl analysis. (author)

Candidate coffee reference material for element content: production and certification schemes adopted at CENA/USP

Energy Technology Data Exchange (ETDEWEB)

Tagliaferro, Fabio Sileno; Fernandes, Elisabete A. de Nadai; Bacchi, Marcio Arruda; Franca, Elvis Joacir de [Centro de Energia Nuclear na Agricultura (CENA/USP), Piracicaba, SP (Brazil). Lab. de Radioisotopos], e-mail: fabiotag@cena.usp.br, e-mail: lis@cena.usp.br, e-mail: mabacchi@cena.usp.br, e-mail: ejfranca@cena.usp.br; Bode, Peter; Bacchi, Marcio Arruda; Franca, Elvis Joacir de [Delft University of Technology, Delft (Netherlands). Interfaculty Reactor Inst.], e-mail: P.Bode@iri.tudelft.nl

2003-07-01

Certified reference materials (CRMs) play a fundamental role in analytical chemistry establishing the traceability of measurement results and assuring accuracy and reliability. In spite of the huge importance of measurements in the food sector, Brazil does not produce CRMs to supply the demand. Consequently the acquisition of CRMs depends on imports at high costs. The coffee sector needs CRMs, however there is no material that represents the coffee composition. Since 1998, the Laboratorio de Radioisotopos (LRi) of CENA/USP has been involved in analysis of coffee. During this period, knowledge has been accumulated about several aspects of coffee, such as system of cultivation, elemental composition, homogeneity of the material, possible contaminants and physical properties of beans. Concomitantly, LRi has concentrated efforts in the field of metrology in chemistry, and now all this expertise is being used as the basis for the production of a coffee certified reference material (CRM) for inorganic element content. The scheme developed for the preparation and certification of coffee RM relies on the ISO Guides 34 and 35. The approaches for selection, collection and preparation of the material, moisture determination method, homogeneity testing, certification and long-term stability testing are discussed and a time frame for the expected accomplishments is provided. (author)

Candidate coffee reference material for element content: production and certification schemes adopted at CENA/USP

International Nuclear Information System (INIS)

Tagliaferro, Fabio Sileno; Fernandes, Elisabete A. de Nadai; Bacchi, Marcio Arruda; Franca, Elvis Joacir de; Bode, Peter; Bacchi, Marcio Arruda; Franca, Elvis Joacir de

2003-01-01

Certified reference materials (CRMs) play a fundamental role in analytical chemistry establishing the traceability of measurement results and assuring accuracy and reliability. In spite of the huge importance of measurements in the food sector, Brazil does not produce CRMs to supply the demand. Consequently the acquisition of CRMs depends on imports at high costs. The coffee sector needs CRMs, however there is no material that represents the coffee composition. Since 1998, the Laboratorio de Radioisotopos (LRi) of CENA/USP has been involved in analysis of coffee. During this period, knowledge has been accumulated about several aspects of coffee, such as system of cultivation, elemental composition, homogeneity of the material, possible contaminants and physical properties of beans. Concomitantly, LRi has concentrated efforts in the field of metrology in chemistry, and now all this expertise is being used as the basis for the production of a coffee certified reference material (CRM) for inorganic element content. The scheme developed for the preparation and certification of coffee RM relies on the ISO Guides 34 and 35. The approaches for selection, collection and preparation of the material, moisture determination method, homogeneity testing, certification and long-term stability testing are discussed and a time frame for the expected accomplishments is provided. (author)

Preparation and characterization of the fish reference material

International Nuclear Information System (INIS)

Ulrich, Joao Cristiano

2011-01-01

The certified reference materials (CRMs) play an important role in obtaining measurement results traceable to the International System of Units, through an unbroken chain of comparisons. Thus, the demand for new certified reference materials (CRMs) increases every day in all areas of knowledge. The availability of reference materials, mainly in Brazil is still incipient, given that the demand far exceeds the available variety of these materials. The amount of certified reference materials available in the country is insufficient to meet the need of the scientific community and demands for development of new methodologies. Among the many areas in need of reference materials, we highlight the importance for the food trade balance for these products within the country. The certification of food products, intended both for export and for domestic consumption, requires analysis methods that provide precise and accurate results to ensure product quality. This paper describes the preparation and certification of a reference material in the fish matrix in mercury and methylmercury. The study brings together since the stage of material selection, preparation, development of homogeneity and stability studies and characterization. The certification was performed by means of measurements using two analytical techniques, flow injection analysis - cold vapor atomic absorption spectrometry (FIA-CV-AAS) and isotope dilution applied to mass spectrometry (IDMS), which is a primary method. In this work the standards of the ISO 30 (ABNT 30-34) and ISO Guide 35 was used as the basis for the preparation and characterization of the material. For the calculation of uncertainties was used the GUM and Eurachem guide. As a result, was produced and certified a lot of material in relation to the concentration of mercury (Hg = 0.271 ± 0.057 mg g -1 ) and methylmercury (MeHg = 0.245 ± 0.038 mg g -1 ), and informational values of lead and arsenic. (author)

Homogeneity and evaluation of the new NIST leaf certified reference materials

International Nuclear Information System (INIS)

Becker, D.A.

1990-01-01

The NIST has produced and is in the process of certifying two new leaf CRMs, SRM1515 Apple Leaves and SRM 1547 Peach Leaves, as replacements for the no longer available NBS Orchard Leaves and the almost depleted Citrus Leaves. These two new materials have been processed and are being thoroughly evaluated and should provide the most advanced natural matrix botanical trace-element reference materials available. Caution should be used in determining a basis weight (drying) for these CRMs because of their very fine particle size. Homogeneity has been established by instrumental neutron activation analysis on both leaf materials for five elements, to date, to better than 1.5% (1 s) for 100-mg sample sizes

A new certified reference material for benzene measurement in air on a sorbent tube: development and proficiency testing

Energy Technology Data Exchange (ETDEWEB)

Caurant, A. [Laboratoire National de Metrologie et d' Essais, Paris (France); Universite Paris 12 et CNRS (UMR 7583), Faculte des Sciences et Technologie, Laboratoire Inter-universitaire des Systemes Atmospheriques, Unite Mixte de Recherche Universite Paris 7 (France); Lalere, B.; Schbath, M.C.; Stumpf, C.; Sutour, C.; Mace, T.; Vaslin-Reimann, S. [Laboratoire National de Metrologie et d' Essais, Paris (France); Quisefit, J.P.; Doussin, J.F. [Universite Paris 12 et CNRS (UMR 7583), Faculte des Sciences et Technologie, Laboratoire Inter-universitaire des Systemes Atmospheriques, Unite Mixte de Recherche Universite Paris 7 (France)

2010-11-15

A certified matrix reference material (CRM) for the measurement of benzene in ambient air has been developed at Laboratoire National de Metrologie et d'Essais. The production of these CRMs was conducted using a gravimetric method fully traceable to the International System of Units. The CRMs were prepared by sampling an accurate mass of a gaseous primary reference material of benzene, using a high-precision laminar flowmeter and a mass flow controller, with a PerkinElmer sampler filled with Carbopack trademark X sorbent. The relative standard deviations obtained for the preparation of a batch of 20 tubes loaded with 500 ng of benzene were below 0.2%. Each CRM is considered independent from the others and with its own certified value and an expanded uncertainty estimated to be within 0.5%, lower than the uncertainties of benzene CRMs already available worldwide. The stability of these materials was also established up to 12 months. These CRMs were implemented during proficiency testing, to evaluate the analytical performances of seven French laboratories involved in benzene air monitoring. (orig.)

Final report on CCQM-K79: Comparison of value-assigned CRMs and PT materials: Ethanol in aqueous matrix

Science.gov (United States)

Hein, Sebastian; Philipp, Rosemarie; Duewer, David L.; Gasca Aragon, Hugo; Lippa, Katrice A.; Toman, Blaza

2013-01-01

The 2010 CCQM-K79 'Comparison of value-assigned CRMs and PT materials: Ethanol in aqueous media' is the second key comparison directly testing the chemical measurement services provided to customers by National Metrology Institutes (NMIs) and Designated Institutes (DIs). CCQM-K79 compared the assigned ethanol values of proficiency test (PT) and certified reference materials (CRMs) using measurements made on these materials under repeatability conditions. Nine NMIs submitted 27 CRM or value-assigned PT materials for evaluation. These materials represent many of the higher-order reference materials then available for this commercially and forensically important measurand. The assigned ethanol mass fraction in the materials ranged from 0.1 mg/kg to 334 mg/kg. All materials were stored and prepared according the specifications provided by each NMI. Samples were processed and analyzed under repeatability conditions by one analytical team using a gas chromatography with flame ionization detection (GC-FID) method of demonstrated trueness and precision. Given the number of materials and the time required for each analysis, the majority of the measurements were made in two measurement campaigns ('runs'). Due to a shipping delay from one NMI, an unanticipated third campaign was required. In all three campaigns, replicate analyses (three injections of one preparation separated in time) were made for one randomly selected unit of each of the 27 materials. Nine of the 27 materials were gravimetrically diluted before measurement to provide solutions with ethanol mass fraction in the established linear range of the GC-FID method. The repeatability measurement value for each analyzed solution was estimated as the mean of all replicate values. The within- and between-campaign variance components were estimated using one-way ANOVA. Markov Chain Monte Carlo Bayesian analysis was used to estimate 95% level-of-confidence coverage intervals for the mean values. Uncertainty

CETAMA contribution to safeguards and nuclear forensic analysis based on nuclear reference materials

International Nuclear Information System (INIS)

Roudil, D.; Rigaux, C.; Rivier, C.; Hubinois, J.C.; Aufore, L.

2012-01-01

Measurement quality is crucial for the safety of nuclear facilities: nuclear reference materials (CRM) and interlaboratory programs (ILC), beyond the assessment of analytical measurement quality, play an important role. In the nuclear field, the CETAMA proposes suitable scientific and technical developments, in particular the preparation and certification of CRM used either as analytical standards or as reference samples for ILCs. The growing emphasis on nuclear forensic measurements will require some re-certification of old CRMs. But the future analytical challenges of meeting nuclear fuel cycle needs and of ensuring safeguard performance improvements will also concern the future CRMs. (authors)

Vision of new generation CRMs for QC of microanalysis

International Nuclear Information System (INIS)

Tian Weizhi

2005-01-01

Direct analysis of ever smaller solid samples has become one of the trends in modern analytical science, in coping with the increasing requirements from life, materials, environment, and other frontier scientific fields. Due to the lack of natural matrix CRMs certified at matched sample size levels, however, quantitative calibration and quality control have long been a bottleneck of microanalysis. CRMs of new generation are therefore called for to make solid sampling microanalysis an accurately quantitative and quality-controllable technique. In this paper, an approach is proposed to use a combination of several nuclear analytical techniques in the certification of RMs suitable for QC of analyses at sub-ng sample size levels. The technical procedures, the major problems, and the possible format of certificates of the new generation CRMs, and the outliik of the establishment of QC system for microanalysis are described. The CRMs of current generation have played an important role in the quality of analysis, especially trace analysis, and in turn in the development of related scientific fields in 20 th century. It may be reasonably predicted that the new generation CRMs will play the similar role in the quality of microanalysis, and in turn in relevant frontier scientific fields in 21 st century. Nuclear analytical techniques have made, and will continue to make, unique contributions to both generations of CRMs.

Certified reference materials and reference methods for nuclear safeguards and security.

Science.gov (United States)

Jakopič, R; Sturm, M; Kraiem, M; Richter, S; Aregbe, Y

2013-11-01

Confidence in comparability and reliability of measurement results in nuclear material and environmental sample analysis are established via certified reference materials (CRMs), reference measurements, and inter-laboratory comparisons (ILCs). Increased needs for quality control tools in proliferation resistance, environmental sample analysis, development of measurement capabilities over the years and progress in modern analytical techniques are the main reasons for the development of new reference materials and reference methods for nuclear safeguards and security. The Institute for Reference Materials and Measurements (IRMM) prepares and certifices large quantities of the so-called "large-sized dried" (LSD) spikes for accurate measurement of the uranium and plutonium content in dissolved nuclear fuel solutions by isotope dilution mass spectrometry (IDMS) and also develops particle reference materials applied for the detection of nuclear signatures in environmental samples. IRMM is currently replacing some of its exhausted stocks of CRMs with new ones whose specifications are up-to-date and tailored for the demands of modern analytical techniques. Some of the existing materials will be re-measured to improve the uncertainties associated with their certified values, and to enable laboratories to reduce their combined measurement uncertainty. Safeguards involve the quantitative verification by independent measurements so that no nuclear material is diverted from its intended peaceful use. Safeguards authorities pay particular attention to plutonium and the uranium isotope (235)U, indicating the so-called 'enrichment', in nuclear material and in environmental samples. In addition to the verification of the major ratios, n((235)U)/n((238)U) and n((240)Pu)/n((239)Pu), the minor ratios of the less abundant uranium and plutonium isotopes contain valuable information about the origin and the 'history' of material used for commercial or possibly clandestine purposes, and

The urgent requirement for new radioanalytical certified reference materials for nuclear safeguards, forensics, and consequence management

International Nuclear Information System (INIS)

Inn, K.G.W.; Martin Johnson, Jr.C.; Warren Oldham; Lav Tandon; Simon Jerome; Thomas Schaaff; Robert Jones; Daniel Mackney; Pam MacKill; Brett Palmer

2013-01-01

A multi-agency workshop was held from 25 to 27 August 2009, at the National Institute of Standards and Technology (NIST), to identify and prioritize the development of radioanalytical Certified Reference Materials (CRMs, generally provided by National Metrology Institutes; Standard Reference Materials, a CRM issued by NIST) for field and laboratory nuclear measurement methods to be used to assess the consequences of a domestic or international nuclear event. Without these CRMs, policy makers concerned with detecting proliferation and trafficking of nuclear materials, attribution and retribution following a nuclear event, and public health consequences of a nuclear event would have difficulty making decisions based on analytical data that would stand up to scientific, public, and judicial scrutiny. The workshop concentrated on three areas: post-incident Improvised Nuclear Device (IND) nuclear forensics, safeguard materials characterization, and consequence management for an IND or a Radiological Dispersion Device detonation scenario. The workshop identified specific CRM requirements to fulfill the needs for these three measurement communities. Of highest priority are: (1) isotope dilution mass spectrometry standards, specifically 233 U, 236 gNp, 244 Pu, and 243 Am, used for quantitative analysis of the respective elements that are in critically short supply and in urgent need of replenishment and certification; (2) CRMs that are urgently needed for post-detonation debris analysis of actinides and fission fragments, and (3) CRMs used for destructive and nondestructive analyses for safeguards measurements, and radioisotopes of interest in environmental matrices. (author)

Preparation and characterization of the fish reference material; Preparacao e caracterizacao de um material de referencia de peixe

Energy Technology Data Exchange (ETDEWEB)

Ulrich, Joao Cristiano

2011-07-01

The certified reference materials (CRMs) play an important role in obtaining measurement results traceable to the International System of Units, through an unbroken chain of comparisons. Thus, the demand for new certified reference materials (CRMs) increases every day in all areas of knowledge. The availability of reference materials, mainly in Brazil is still incipient, given that the demand far exceeds the available variety of these materials. The amount of certified reference materials available in the country is insufficient to meet the need of the scientific community and demands for development of new methodologies. Among the many areas in need of reference materials, we highlight the importance for the food trade balance for these products within the country. The certification of food products, intended both for export and for domestic consumption, requires analysis methods that provide precise and accurate results to ensure product quality. This paper describes the preparation and certification of a reference material in the fish matrix in mercury and methylmercury. The study brings together since the stage of material selection, preparation, development of homogeneity and stability studies and characterization. The certification was performed by means of measurements using two analytical techniques, flow injection analysis - cold vapor atomic absorption spectrometry (FIA-CV-AAS) and isotope dilution applied to mass spectrometry (IDMS), which is a primary method. In this work the standards of the ISO 30 (ABNT 30-34) and ISO Guide 35 was used as the basis for the preparation and characterization of the material. For the calculation of uncertainties was used the GUM and Eurachem guide. As a result, was produced and certified a lot of material in relation to the concentration of mercury (Hg = 0.271 {+-} 0.057 mg g{sup -1}) and methylmercury (MeHg = 0.245 {+-} 0.038 mg g{sup -1}), and informational values of lead and arsenic. (author)

Production of candidate natural matrix reference materials for micro-analytical techniques

International Nuclear Information System (INIS)

Zeisler, R.; Fajgelj, A.; Zeiller, E.

2002-01-01

Homogeneity is considered to be the most vital prerequisite for a certified reference material (CRM); more stringent requirements exist for the analysis of small subsamples. Many of the natural matrix CRMs are prepared from bulk samples by grinding and milling them to a certain particle size, which is expected to provide a more homogenous material; however recommended sample sizes for biological and environmental reference materials are found to be more than 100 mg. Since the milling of materials is costly and has some drawbacks, natural materials that already occur as small particles such as air particulate matter, certain sediments, and cellular biological materials may form the basis of the required reference materials. The nature of these materials, i.e. naturally occurring particles, may provide ideal model reference material. We describe here the production of the materials and preliminary tests, the evaluation for the micro-analytical techniques

NAA study on homogeneity of reference materials and their suitability for microanalytical techniques

International Nuclear Information System (INIS)

Dybczynski, R.; Danko, B.; Polkowska-Motrenko, H.

2000-01-01

Homogeneity of the existing (Virginia Tobacco Leaves CTA-VTL-2 (ICHTJ), Apatite Concentrate CTA-AC-1 (ICHTJ), Fine Fly Ash CTA-FFA-1 (ICHTJ)) and candidate certified reference materials (CRMs) (IAEA-338 Lichen, IAEA-413 Algae, Spruce Shoots RMF II (Germany)) was studied by neutron activation analysis (NAA). Several samples of small mass (ca. 1 or 10 mg) taken from various containers were analyzed by instrumental NAA and the results for several elements were compared by Fishers's test and t-test with analogous series of results for samples taken from one container. In the second approach, sampling variance was estimated for some elements from overall variance and the components of analytical variance. The results were interpreted with the aid of Ingamells' sampling constant. Particle size distribution of the reference materials was also measured by several techniques. In addition quantitative determinations for some elements were performed and results compared with the certified values. The results of the present study were discussed with reference to suitability of CRMs to microanalytical techniques. It was pointed out that the term 'microanalysis' itself is not always unequivocally understood and used. (author)

Speciation of dimethylarsinyl-riboside derivatives (arsenosugars) in marine reference materials by HPLC-ICP-MS

DEFF Research Database (Denmark)

Larsen, Erik Huusfeldt

1995-01-01

(cf. Table 2) were present in shellfish certified reference materials (CRMs) and in a lobster hepatopancreas CRM. The concentration of the two arsenosugars in the shellfish samples amounts to 18% of the total arsenic as compared to arsenobetaine at 9–13% and dimethylarsinate at 4–9% of the total...

Evaluation of ABS resin disk certified reference materials for heavy metal analysis by x-ray fluorescence analysis

International Nuclear Information System (INIS)

Ohata, Masaki; Kidokoro, Toshihiro; Kurahashi, Masayasu; Hioki, Akiharu

2010-01-01

ABS resin disk certified reference materials (CRMs) for heavy-metal analysis (NMIJ CRM 8105-a, NMIJ CRM 8106-a, NMIJ CRM 8115-a and NMIJ CRM 8116-a) were evaluated using an energy dispersive X-ray fluorescence (ED-XRF) analysis. The homogeneities of elements for both among-disks and within-disk were evaluated by ED-XRF analysis without any sample pre-treatment, which were similar to those evaluated by ICP-MS analysis after a sample digenstion procedure. The normalized XRF sensitivities for Cd, Cr and Pb in different ABS resin disk CRMs were compared, and the differences among them for those ABS resin disks that have similar matrices were observed. Moreover, Hg in those ABS resin disk CRMs was stable for long-term X-ray irradiation during ED-XRF analysis. (author)

Lead isotopic compositions of environmental certified reference materials for an inter-laboratory comparison of lead isotope analysis

International Nuclear Information System (INIS)

Aung, Nyein Nyein; Uryu, Tsutomu; Yoshinaga, Jun

2004-01-01

Lead isotope ratios, viz. 207 Pb/ 206 Pb and 208 Pb/ 206 Pb, of the commercially available certified reference materials (CRMs) issued in Japan are presented with an objective to provide a data set, which will be useful for the quality assurance of analytical procedures, instrumental performance and method validation of the laboratories involved in environmental lead isotope ratio analysis. The analytical method used in the present study was inductively coupled plasma quadrupole mass spectrometry (ICPQMS) presented by acid digestion and with/without chemical separation of lead from the matrix. The precision of the measurements in terms of the relative standard deviation (RSD) of triplicated analyses was 0.19% and 0.14%, for 207 Pb/ 206 Pb and 208 Pb/ 206 Pb, respectively. The trueness of lead isotope ratio measurements of the present study was tested with a few CRMs, which have been analyzed by other analytical methods and reported in various literature. The lead isotopic ratios of 18 environmental matrix CRMs (including 6 CRMs analyzed for our method validation) are presented and the distribution of their ratios is briefly discussed. (author)

Preparation and evaluation of reference materials for accountancy analysis. (1) Preparation and evaluation method

International Nuclear Information System (INIS)

Takamatsu, Mai; Kacchi, Tomokazu; Murakami, Toshiki; Ai, Hironobu; Sumi, Mika; Abe, Katsuo; Kageyama, Tomio; Nakazawa, Hiroaki

2009-01-01

Isotope dilution mass spectrometry method used for the accountancy analysis at nuclear fuel facilities requires the standard materials called LSD (Large Size Dried) spike. Generally, LSD spikes are prepared from certified reference materials (CRMs) which supplied from foreign laboratories. However, the difficulty of Pu CRM importation is increasing. It is important for safeguards to attain and continue high reliable accountancy analysis and stable securing of LSD spike is essential. Therefore, in order to conserve CRMs, several types of LSD spike were prepared under collaboration work between JAEA and JNFL, such as the amount of nuclear material in one LSD spike is decreased and others. Practical test with actual samples were performed at JNFL Rokkasho reprocessing plant, and those results were compared with the results obtained by using LSD spike which supplied from foreign laboratory. Preparation and verification analysis of LSD spikes and evaluation of uncertainty based on ISO-GUM will be presented. (author)

The importance of reference materials in doping-control analysis.

Science.gov (United States)

Mackay, Lindsey G; Kazlauskas, Rymantas

2011-08-01

Currently a large range of pure substance reference materials are available for calibration of doping-control methods. These materials enable traceability to the International System of Units (SI) for the results generated by World Anti-Doping Agency (WADA)-accredited laboratories. Only a small number of prohibited substances have threshold limits for which quantification is highly important. For these analytes only the highest quality reference materials that are available should be used. Many prohibited substances have no threshold limits and reference materials provide essential identity confirmation. For these reference materials the correct identity is critical and the methods used to assess identity in these cases should be critically evaluated. There is still a lack of certified matrix reference materials to support many aspects of doping analysis. However, in key areas a range of urine matrix materials have been produced for substances with threshold limits, for example 19-norandrosterone and testosterone/epitestosterone (T/E) ratio. These matrix-certified reference materials (CRMs) are an excellent independent means of checking method recovery and bias and will typically be used in method validation and then regularly as quality-control checks. They can be particularly important in the analysis of samples close to threshold limits, in which measurement accuracy becomes critical. Some reference materials for isotope ratio mass spectrometry (IRMS) analysis are available and a matrix material certified for steroid delta values is currently under production. In other new areas, for example the Athlete Biological Passport, peptide hormone testing, designer steroids, and gene doping, reference material needs still need to be thoroughly assessed and prioritised.

Determination of rare earth and uranium in reference biological materials certified by the method of neutron activation analysis

International Nuclear Information System (INIS)

Pereira, Lais H.P.; Saiki, Mitiko

2013-01-01

The objective of this study was to evaluate the precision and accuracy of the determinations of Sc, La, Ce, Nd, Sm, Eu, Tb, Yb, Lu and U in certified reference materials (CRMs). To solve the problem of interference from fission products of U in the determination of lanthanides were obtained correction factors for this interference for 140 La, 141 Ce, 143 Ce, 153 Sm and 147 Nd. The experimental procedure of Neutron Activation Analysis consisted of irradiating aliquots of each of the CRMs with synthetic standards of elements under thermal neutron flux of the IEA-R1 nuclear reactor, followed by gamma-ray spectrometry using a high-resolution hyperpurity GE detector. The analyzes of CRMs indicate good accuracy and precision of results, demonstrating the feasibility of applying of established procedure in NAA of elements studied in organic vegetable matrices

Collaborative analysis for certification of zirconium and zirconium base alloy reference materials JAERI-Z11 to Z16

International Nuclear Information System (INIS)

1985-03-01

The second Sub-Committee on Zircaloy Analysis was organized in April 1978, under the Committee on Analytical Chemistry on Nuclear Fuels and Reactor Materials, JAERI, for the renewal of zirconium and zirconium base alloy certified reference materials (CRMs). The Sub-Committee carried out collaborative analysis among 13 participating laboratories for the certification of the CRMs, JAERI-Z11 to Z18, after development, improvement and evaluation of analytical methods during the period of May 1978 to June 1982. As the result of the collaborative analysis, the certified value was given for 18 elements (Sn, Fe, Ni, Cr, B, Cd, U, Cu, Co, Mn, Pb, Al, Ti, Si, Mo, W, Hf, C) in the CRMs. The first part of this report includes general discussion, the second part principles of certification, the third part development and verification of analytical methods, and the fourth part evaluation of analytical results on 17 elements. Preparation of Z11 to Z18, and certification for carbon in JAERI-Z17 and Z18 were reported separately in JAERI-M 83-241 and M 83-035, respectively. (author)

Preparation and certification of certified reference materials JAERI-Z21, Z22 and Z23 for analysis of zirconium and its alloys

International Nuclear Information System (INIS)

Takashima, Kyoichiro

1991-03-01

The Sub-Committee on Chemical Analysis of Nuclear Materials was organized in April 1987, under the Committee on Analytical Chemistry of Nuclear Fuels and Reactor Materials, JAERI, for renewal of certified reference materials of zirconium base alloys and zirconium metal. Collaborative analysis was carried out among ten participating laboratories for the certification of the JAERI CRMs Z21 to Z23. As a results of the collaborative works, the certified values for sixteen elements (Sn, Fe, Ni, Cr, Hf, Al, Si, Co, Cu, Ti, Mn, Pb, U, Cd, B and W) in the CRMs were given. In this report, preparation of raw materials, homogeneity test, chemical analysis for certification by collaborative works during April 1987 to March 1990 are described. (author)

Certified reference materials for radionuclides in Bikini Atoll sediment (IAEA-410) and Pacific Ocean sediment (IAEA-412)

DEFF Research Database (Denmark)

Pham, M. K.; van Beek, P.; Carvalho, F. P.

2016-01-01

The preparation and characterization of certified reference materials (CRMs) for radionuclide content in sediments collected offshore of Bikini Atoll (IAEA-410) and in the open northwest Pacific Ocean (IAEA-412) are described and the results of the certification process are presented. The certified...... radionuclides include: 40K, 210Pb (210Po), 226Ra, 228Ra, 228Th, 232Th, 234U, 238U, 239Pu, 239+240Pu and 241Am for IAEA-410 and 40K, 137Cs, 210Pb (210Po), 226Ra, 228Ra, 228Th, 232Th, 235U, 238U, 239Pu, 240Pu and 239+240Pu for IAEA-412. The CRMs can be used for quality assurance and quality control purposes...

Final certification of two new reference materials for inorganic trace analysis

International Nuclear Information System (INIS)

Dybczynski, R.; Danko, B.; Kulisa, K.; Chajduk-Maleszewska, E.; Polkowska-Motrenko, H.; Samczynski, Z.; Szopa, Z.

2004-01-01

Two new biological reference materials for inorganic trace analysis: Tea Leaves (INCT-TL-1) and Mixed Polish Herbs (INCT-MPH-2) were prepared and certified at the Institute of Nuclear Chemistry and Technology (INCT), Warsaw, employing the general strategy of the preparation and certification of CRMs developed in INCT. For both materials ca 40 kg of ground, sieved and carefully homogenized fraction of nominal particle size ≤ 67 mm was obtained. Homogeneity of the materials studied by INAA was shown to be good for samples of masses: m ≥ 100 mg but further investigations indicate that for most of elements these materials can be considered homogeneous down to masses of ca 5 mg or perhaps even lower. The certification was based on results of a worldwide interlaboratory comparison, in which 109 laboratories from 19 countries participated. The results of the analysis of a CRM, which was sent and analyzed along with intercomparison samples and the identity of which was known only to the organizers, were utilized in the process of certification. In addition selected elements were analyzed also by definitive methods based on RNAA. The content of more than 30 elements could be certified in each of the new CRMs. Analytical uncertainties and stability uncertainties were quantified to arrive at combined uncertainties of the certified values. In addition information values were provided for some other elements. (author)

Development of a new certified reference material of diosgenin using mass balance approach and Coulometric titration method.

Science.gov (United States)

Gong, Ningbo; Zhang, Baoxi; Hu, Fan; Du, Hui; Du, Guanhua; Gao, Zhaolin; Lu, Yang

2014-12-01

Certified reference materials (CRMs) can be used as a valuable tool to validate the trueness of measurement methods and to establish metrological traceability of analytical results. Diosgenin has been selected as a candidate reference material. Characterization of the material relied on two different methods, mass balance method and Coulometric titration method (CT). The certified value of diosgenin CRM is 99.80% with an expanded uncertainty of 0.37% (k=2). The new CRM of diosgenin can be used to validate analytical methods, improve the accuracy of measurement data and control the quality of diosgenin in relevant pharmaceutical formulations. Copyright © 2014 Elsevier Inc. All rights reserved.

Survey of total error of precipitation and homogeneous HDL-cholesterol methods and simultaneous evaluation of lyophilized saccharose-containing candidate reference materials for HDL-cholesterol

NARCIS (Netherlands)

C.M. Cobbaert (Christa); H. Baadenhuijsen; L. Zwang (Louwerens); C.W. Weykamp; P.N. Demacker; P.G.H. Mulder (Paul)

1999-01-01

textabstractBACKGROUND: Standardization of HDL-cholesterol is needed for risk assessment. We assessed for the first time the accuracy of HDL-cholesterol testing in The Netherlands and evaluated 11 candidate reference materials (CRMs). METHODS: The total error (TE) of

Critical outlook and trends for environmental reference materials at the Measurements & Testing Generic Activity (European Commission).

Science.gov (United States)

Quevauviller, P; Bennink, D; Bøwadt, S

2001-05-01

It is now well recognised that the quality control (QC) of all types of analyses, including environmental analyses depends on the appropriate use of reference materials. One of the ways to check the accuracy of methods is based on the use of Certified Reference Materials (CRMs), whereas other types of (not certified) Reference Materials (RMs) are used for routine quality control (establishment of control charts) and interlaboratory testing (e.g. proficiency testing). The perception of these materials, in particular with respect to their production and use, differs widely according to various perspectives (e.g. RM producers, routine laboratories, researchers). This review discusses some critical aspects of RM use and production for the QC of environmental analyses and describes the new approach followed by the Measurements & Testing Generic Activity (European Commission) to tackle new research and production needs.

A certified urea reference material (NMIJ CRM 6006-a) as a reliable calibrant for the elemental analyses of amino acids and food samples.

Science.gov (United States)

Itoh, Nobuyasu; Yamazaki, Taichi; Sato, Ayako; Numata, Masahiko; Takatsu, Akiko

2014-01-01

We examined the reliability of a certified reference material (CRM) for urea (NMIJ CRM 6006-a) as a calibrant for N, C, and H in elemental analyzers. Only the N content for this CRM is provided as an indicative value. To estimate the C and H contents of the urea CRM, we took into account the purity of the urea and the presence of other identified impurities. When we examined the use of various masses of the calibrant (0.2 to 2 mg), we unexpectedly observed low signal intensities for small masses of H and N, but these plateaued at about 2 mg. We therefore analyzed four amino acid CRMs and four food CRMs on a 2-mg scale with the urea CRM as the calibrant. For the amino acid CRMs, the differences in the analytical and theoretical contents (≤0.0026 kg/kg) were acceptable with good repeatability (≤0.0013 kg/kg in standard deviation; n = 4). For food CRMs, comparable repeatabilities to those obtained with amino acid CRMs (≤0.0025 kg/kg in standard deviation; n = 4) were obtained. The urea CRM can therefore be used as a reliable calibrant for C, H, and N in an elemental analyzer.

Comparison of relative INAA and k0-INAA using soil and sediment reference materials

International Nuclear Information System (INIS)

Jacimovic, R.

2014-01-01

The objective of this work was to compare the results obtained by the relative INAA and k 0 -INAA methods for the same input parameters (sample mass, nuclear data, net peak area for the same gamma line and the same measurement and same cooling and measurement times). In total eight environmental soil and sediment reference materials (RM) or certified reference materials (CRM) from different producers were analysed. In this work only the recommended or certified values were considered, allowing comparison of the two methods for 30 elements. The results point out that k 0 -INAA possesses superior qualities compared to relative INAA, being insensitive to flux gradients, and independent of recommended/certified values in RMs/CRMs, often used as standards in relative INAA. (author)

Testing the homogeneity of candidate reference materials by solid sampling - AAS and INAA

International Nuclear Information System (INIS)

Rossbach, M.; Grobecker, K.-H.

2002-01-01

The necessity to quantify a natural material's homogeneity with respect to its elemental distribution prior to chemical analysis of a given aliquot is emphasised. Available instruments and methods to obtain the relevant information are described. Additionally the calculation of element specific, relative homogeneity factors, H E , and of a minimum sample mass M 5% to achieve 5% precision on a 95% confidence level is given. Especially, in the production and certification of Certified Reference Materials (CRMs) this characteristic information should be determined in order to provide the user with additional inherent properties of the CRM to enable more economical use of the expensive material and to evaluate further systematic bias of the applied analytical technique. (author)

Determination of Al, Si and P in certified reference materials by Instrumental Neutron Activation Analysis

Energy Technology Data Exchange (ETDEWEB)

Noyori, Amanda; Saiki, Mitiko, E-mail: anoyori@gmail.com, E-mail: mitiko@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

2017-11-01

Neutron analysis activation is not commonly used for aluminum, phosphorus and silicon determination, due to the difficulty to obtain reliable results. In this study, Al was determined by measuring {sup 28}Al and the contribution of P and Si due to {sup 28}Al formed in {sup 31}P(n,α){sup 28}Al and {sup 28}Si(n,p){sup 28}Al reactions were corrected using correction factors determined experimentally. Phosphorus was determined by measuring {sup 32}P (pure beta emitter) formed in reaction {sup 31}P(n,γ){sup 32}P. Silicon was determined by epithermal neutron analysis activation (ENAA) and measuring {sup 29}Al radionuclide formed in {sup 29}Si(n,p){sup 29}Al reaction. Aliquots of certified reference materials (CRMs) and synthetic standards of the elements were irradiated together, using the pneumatic transfer station of IEA-R1 nuclear research reactor. Results obtained for biological and geological CRMs showed good precision and accuracy with |Z-score| < 2 for Al, P and Si determinations. The detection limits for Al, P and Si determinations CRMs were also evaluated. Results obtained in this study demonstrated the viability of applying INAA procedures in the determination of Al, P and Si. (author)

Determination of Al, Si and P in certified reference materials by Instrumental Neutron Activation Analysis

International Nuclear Information System (INIS)

Noyori, Amanda; Saiki, Mitiko

2017-01-01

Neutron analysis activation is not commonly used for aluminum, phosphorus and silicon determination, due to the difficulty to obtain reliable results. In this study, Al was determined by measuring "2"8Al and the contribution of P and Si due to "2"8Al formed in "3"1P(n,α)"2"8Al and "2"8Si(n,p)"2"8Al reactions were corrected using correction factors determined experimentally. Phosphorus was determined by measuring "3"2P (pure beta emitter) formed in reaction "3"1P(n,γ)"3"2P. Silicon was determined by epithermal neutron analysis activation (ENAA) and measuring "2"9Al radionuclide formed in "2"9Si(n,p)"2"9Al reaction. Aliquots of certified reference materials (CRMs) and synthetic standards of the elements were irradiated together, using the pneumatic transfer station of IEA-R1 nuclear research reactor. Results obtained for biological and geological CRMs showed good precision and accuracy with |Z-score| < 2 for Al, P and Si determinations. The detection limits for Al, P and Si determinations CRMs were also evaluated. Results obtained in this study demonstrated the viability of applying INAA procedures in the determination of Al, P and Si. (author)

The application of HPLC-F and GC-MS to the analysis of selected hydroxy polycylic hydrocarbons in two certified fish bile reference materials

NARCIS (Netherlands)

Jonsson, G.; Beyer, J.; Wells, D.; Ariese, F.

2003-01-01

Four selected hydroxy polycyclic aromatic hydrocarbons (OH-PAHs), 2-hydroxy-naphthalene (2-OH-NPH), 1-hydroxy-phenanthrene (1-OH-PHE), 1-hydroxy-pyrene (1-OH-PYR) and 3-hydroxy-benzo[a]pyrene (3-OH-BaP) have been analysed in two certified fish bile reference materials (CRMs) for exposure monitoring

The application of HPLC-F and GC-MS to the analysis of selected hydroxy polycyclic hydrocarbons in two certified fish bile reference materials

NARCIS (Netherlands)

Jonsson, G.; Beyer, J.; Wells, D.E.; Ariese, F.

2003-01-01

Four selected hydroxy polycyclic aromatic hydrocarbons (OH-PAHs), 2-hydroxy-naphthalene (2-OH-NPH), 1-hydroxy-phenanthrene (1-OH-PHE), 1-hydroxy-pyrene (1-OH-PYR) and 3-hydroxy-benzo[a]pyrene (3-OH-BaP) have been analysed in two certified fish bile reference materials (CRMs) for exposure monitoring

Standard reference material certification: contribution of NAA with a TRIGA reactor

International Nuclear Information System (INIS)

Orvini, E.; Speziali, M.; Salvini, A.; Herborg, C.

2002-01-01

Pavia has cooperative links with the major international agencies devoted to the certification of SRMs or CRMs as the Bureau Communautaire de Reference (BCR), the European Institute for Reference Materials and Measurement (IRMM), the USA National Institute of Standards and Technology (NIST) and the International Atomic Energy Agency (IAEA). During these cooperative works, a large amount of analytical data obtained with NAA has been compared, and meaningful methodological information achieved with respect to accuracy and precision in the analysis of several elements at different concentrations in various matrices. Analytical data on As, Cd, Cr, Co, Cu, Cs, Fe, Zn, K, Sc, U, Th, Al, Sb, Mn, V, Hg, Sr, Rb, Se,Pt, all the Rare Earths and halogens Br, Cl, I, have been obtained and contributed for the final certification

Certified Reference Material for Use in 1H, 31P, and 19F Quantitative NMR, Ensuring Traceability to the International System of Units.

Science.gov (United States)

Rigger, Romana; Rück, Alexander; Hellriegel, Christine; Sauermoser, Robert; Morf, Fabienne; Breitruck, KathrinBreitruck; Obkircher, Markus

2017-09-01

In recent years, quantitative NMR (qNMR) spectroscopy has become one of the most important tools for content determination of organic substances and quantitative evaluation of impurities. Using Certified Reference Materials (CRMs) as internal or external standards, the extensively used qNMR method can be applied for purity determination, including unbroken traceability to the International System of Units (SI). The implementation of qNMR toward new application fields, e.g., metabolomics, environmental analysis, and physiological pathway studies, brings along more complex molecules and systems, thus making use of 1H qNMR challenging. A smart workaround is possible by the use of other NMR active nuclei, namely 31P and 19F. This article presents the development of three classes of qNMR CRMs based on different NMR active nuclei (1H, 31P, and 19F), and the corresponding approaches to establish traceability to the SI through primary CRMs from the National Institute of Standards and Technology and the National Metrology Institute of Japan. These TraceCERT® qNMR CRMs are produced under ISO/IEC 17025 and ISO Guide 34 using high-performance qNMR.

Development of Certified Matrix-Based Reference Material as a Calibrator for Genetically Modified Rice G6H1 Analysis.

Science.gov (United States)

Yang, Yu; Li, Liang; Yang, Hui; Li, Xiaying; Zhang, Xiujie; Xu, Junfeng; Zhang, Dabing; Jin, Wujun; Yang, Litao

2018-04-11

The accurate monitoring and quantification of genetically modified organisms (GMOs) are key points for the implementation of labeling regulations, and a certified reference material (CRM) acts as the scaleplate for quantifying the GM contents of foods/feeds and evaluating a GMO analytical method or equipment. Herein we developed a series of CRMs for transgenic rice event G6H1, which possesses insect-resistant and herbicide-tolerant traits. Three G6H1 CRMs were produced by mixing seed powders obtained from homozygous G6H1 and its recipient cultivar Xiushui 110 at mass ratios of 49.825%, 9.967%, and 4.986%. The between-bottle homogeneity and within-bottle homogeneity were thoroughly evaluated with consistent results. The potential DNA degradation in transportation and shelf life were evaluated with an expiration period of at least 12 months. The property values of three CRMs (G6H1 a , G6H1 b , G6H1 c ) were given as (49.825 ± 0.448) g/kg, (9.967 ± 1.757) g/kg, and (4.986 ± 1.274 g/kg based on mass fraction ratio, respectively. Furthermore, the three CRMs were characterized with values of (5.01 ± 0.08)%, (1.06 ± 0.22)%, and (0.53 ± 0.11)% based on the copy number ratio using the droplet digital PCR method. All results confirmed that the produced G6H1 matrix-based CRMs are of high quality with precise characterization values and can be used as calibrators in GM rice G6H1 inspection and monitoring and in evaluating new analytical methods or devices targeting the G6H1 event.

Development of certified matrix reference materials for quality assurance of screening 134Cs and 137Cs in food

International Nuclear Information System (INIS)

Ishizu, H.; Yamada, T.

2013-01-01

A certified reference material using activated alumina powder certified for activity of 134 Cs and 137 Cs was developed. The results of the verification and the certification are described. The certified reference material can be used for quality assurance of screening activity measurements of 134 Cs and 137 Cs in food/foodstuffs. Commercially available equipments were experimentally tested using the CRM and another CRM including 40 K. The results of these tests are also shown. - Highlights: • CRM of 134 Cs and 137 Cs using activated alumina was developed. • CRM including 134 Cs, 137 Cs and 40 K was also developed. • Results of experimental performance test of commercial inspection equipments using CRMs were shown

BCR: a service to quality assurance in analytical chemistry - some experiences and achievements with regard to reference material preparation

Energy Technology Data Exchange (ETDEWEB)

Griepink, B. (Commission of the European Communities, Measurements and Testing Programme (BCR), Brussels (Belgium)); Quevauviller, P. (Commission of the European Communities, Measurements and Testing Programme (BCR), Brussels (Belgium)); Maier, E.A. (Commission of the European Communities, Measurements and Testing Programme (BCR), Brussels (Belgium)); Vandendriessche, S. (Commission of the European Communities, Measurements and Testing Programme (BCR), Brussels (Belgium))

Despite all efforts to improve the quality of results of measurements, intercomparisons demonstrate a considerable discrepancy. This fact was also shown by many of the round robins organised by the BCR (Commission of the European Communities) on inorganic, speciation, and organic determinations in various environmental matrices. It is clear that further efforts have to be made to improve the state of the art of a wide variety of analyses. This means that the demand for certified reference materials (CRMs) is and will be in constant increase. RMs are required for the validation of methods, for proficiency testing or for training purposes. The production of RMs and CRMs resembling the composition of real matrices poses difficult problems for some compounds and is a challenge for the producers. This paper presents some recent experiences and achievements of the BCR in special cases. (orig.)

Comparison of a static and a dynamic in vitro model to estimate the bioaccessibility of As, Cd, Pb and Hg from food reference materials Fucus sp. (IAEA-140/TM) and Lobster hepatopancreas (TORT-2)

Energy Technology Data Exchange (ETDEWEB)

Torres-Escribano, Silvia [Instituto de Agroquimica y Tecnologia de Alimentos (IATA-CSIC), Apdo. 73, 46100, Burjassot, Valencia (Spain); Denis, Sylvain; Blanquet-Diot, Stephanie [Clermont Universite, Universite d' Auvergne, Centre de Recherche en Nutrition Humaine Auvergne, ERT 18, Conception ingenierie et developpement de l' aliment et du medicament, BP 10448, F-63000 Clermont-Ferrand (France); Calatayud, Marta [Instituto de Agroquimica y Tecnologia de Alimentos (IATA-CSIC), Apdo. 73, 46100, Burjassot, Valencia (Spain); Barrios, Laura [Departamento de Informatica Cientifica (SGAI-CSIC), C/ Pinar 19, 28006 Madrid (Spain); Velez, Dinoraz, E-mail: deni@iata.csic.es [Instituto de Agroquimica y Tecnologia de Alimentos (IATA-CSIC), Apdo. 73, 46100, Burjassot, Valencia (Spain); Alric, Monique [Clermont Universite, Universite d' Auvergne, Centre de Recherche en Nutrition Humaine Auvergne, ERT 18, Conception ingenierie et developpement de l' aliment et du medicament, BP 10448, F-63000 Clermont-Ferrand (France); Montoro, Rosa [Instituto de Agroquimica y Tecnologia de Alimentos (IATA-CSIC), Apdo. 73, 46100, Burjassot, Valencia (Spain)

2011-01-01

Bioaccessibility, the fraction of an element solubilized during gastrointestinal digestion and available for absorption, is a factor that should be considered when evaluating the health risk of contaminants from food. Static and dynamic models that mimic human physiological conditions have been used to evaluate bioaccessibility. This preliminary study compares the bioaccessibility of arsenic (As), cadmium (Cd), lead (Pb) and mercury (Hg) in two food certified reference materials (CRMs) (seaweed: Fucus sp., IAEA-140/TM; Lobster hepatopancreas: TORT-2), using two in vitro gastrointestinal digestion methods: a static method (SM) and a dynamic multicompartment method (TIM-1). There are significant differences (p < 0.05) between the bioaccessible values of As, Cd, Pb and Hg obtained by SM and TIM-1 in the two CRMs. The specific form in which the elements studied are present in the CRM may help to explain the bioaccessibility values obtained. - Research Highlights: {yields}Data are reported for As, Cd, Pb and Hg bioaccessibility from food CRMs. {yields}The static and TIM-1 methods give significantly different bioaccessibility values. {yields}The possible influence of speciation on bioaccessibility is discussed. {yields}To improve bioaccessibility quality data, food reference materials are needed.

Comparison of a static and a dynamic in vitro model to estimate the bioaccessibility of As, Cd, Pb and Hg from food reference materials Fucus sp. (IAEA-140/TM) and Lobster hepatopancreas (TORT-2)

International Nuclear Information System (INIS)

Torres-Escribano, Silvia; Denis, Sylvain; Blanquet-Diot, Stephanie; Calatayud, Marta; Barrios, Laura; Velez, Dinoraz; Alric, Monique; Montoro, Rosa

2011-01-01

Bioaccessibility, the fraction of an element solubilized during gastrointestinal digestion and available for absorption, is a factor that should be considered when evaluating the health risk of contaminants from food. Static and dynamic models that mimic human physiological conditions have been used to evaluate bioaccessibility. This preliminary study compares the bioaccessibility of arsenic (As), cadmium (Cd), lead (Pb) and mercury (Hg) in two food certified reference materials (CRMs) (seaweed: Fucus sp., IAEA-140/TM; Lobster hepatopancreas: TORT-2), using two in vitro gastrointestinal digestion methods: a static method (SM) and a dynamic multicompartment method (TIM-1). There are significant differences (p < 0.05) between the bioaccessible values of As, Cd, Pb and Hg obtained by SM and TIM-1 in the two CRMs. The specific form in which the elements studied are present in the CRM may help to explain the bioaccessibility values obtained. - Research Highlights: →Data are reported for As, Cd, Pb and Hg bioaccessibility from food CRMs. →The static and TIM-1 methods give significantly different bioaccessibility values. →The possible influence of speciation on bioaccessibility is discussed. →To improve bioaccessibility quality data, food reference materials are needed.

Use of INAA in the preparation of a set soil Reference Materials with certified values of total element contents

International Nuclear Information System (INIS)

Kucera, J.; Horakova, J.; Soukal, L.

1997-01-01

A set of certified Reference Materials was prepared consisting of four natural agricultural soils with normal (n) and elevated (e) levels of element contents: CRM 7001 Light Sandy Soil (n), CRM 7002 Light Sandy Soil (e), CRM 7003 Silty Clay Loam (n), and CRM 7004 Loam (e). In these materials, certified and/or information values of the total contents of the elements As, Ba, Be, Cd, Co, Cr, Cu, Hg, Mn, Ni, Pb, V and Zn, and their fractions extractable by aqua regia, boiling and cold 2M nitric acid were derived from an interlaboratory comparison in which 28 laboratories participated. Highly precise and accurate procedures of instrumental neutron activation analysis (INAA) were employed for homogeneity testing and also for certification of the total element contents. For comparation purposes, NIST SRM-2704 Buffalo River Sediment was analyzed by INAA, as well. The INAA results obtained compared very well with the certified and/or information values for four soil CRMs and also with NIST values for SRM-2704. From this agreement, a very high reliability of the new soil CRMs can be inferred. (author)

Suitability of NAA for certification of reference materials for multielements

International Nuclear Information System (INIS)

Tian Weizhi; Ni Bangfa; Wang Pingsheng; Nie Huiling

2000-01-01

Certifications of trace elements in existing CRMs, especially biological CRMs, are far from satisfactory. Neutron activation analysis (NAA) for its inherent advantages combined with newly established parametric standardization, may contribute to improve this situation. The continuing progress of the hybrid extended k 0 -relative NAA technique developed in our laboratory is discussed. Examples are given to show the reliability of the method in certification of multielements. RNAA is still one of the best methods, or even the method of choice, in analysis at sub-μg/g concentration levels. The suitability of the technique for this purpose has been studied through the determination of rare earth elements at ng/g concentration level in two Chinese biological CRMs using both RNAA and ICPMS. Sampling behaviors of multielements in CRMs have been studied by INAA in an effort to develop CRMs suitable for analysis with small sample sizes. (author)

Determination of polychlorinated dibenzo-p-dioxin and dibenzofuran congeners in air particulate and marine sediment standard reference materials (SRMs).

Science.gov (United States)

Chiu, C H; Turle, R; Poole, G; Thibert, B; Brubaker, W W; Schantz, M M; Wise, S A

2001-02-01

Due to the limited number of environmental matrix certified reference materials (CRMs) with assigned values for natural levels of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs), an interlaboratory study was undertaken by the National Institute of Standards and Technology (NIST) and Environment Canada to establish reference concentration values for selected PCDD/Fs in two well-characterized NIST Standard Reference Materials (SRMs): SRM 1649a (Urban Dust) and SRM 1944 (New York/New Jersey Waterway Sediment). Results from 14 laboratories were used to provide reference values for the seventeen 2, 3, 7, 8-substituted PCDD/F congeners, the totals for individual tetra- through hepta-substituted PCDD/F homologues, and the total amount of tetra- through hepta-substituted PCDD/Fs. The mass fractions for the individual 2, 3, 7, 8-substituted congeners range from approximately 0.01 microg/kg to 7 microg/kg dry mass.

Application of reference materials for quality assessment in neutron activation analysis

International Nuclear Information System (INIS)

Obrusnik, I.; Eckschlager, K.

1993-01-01

It is generally accepted that an analytical procedure can be regarded as an information production system yielding information on the composition of the analyzed sample. Thus, information theory can be useful and the quantities characterizing the information properties of an analytical method may be applied not only as evaluation criteria but also as objective functions in the optimization. The usability of information theory is demonstrated on the example of neutron activation analysis. Both precision and bias of NAA results are taken into account together with the possible use of reference materials for quality assessment. The influence of the above-mentioned parameters on information properties such as information gain and profitability of NAA results is discussed in detail. It has been proved that information theory is especially useful in choosing suitable reference materials for the quality assessment of routine analytical procedures not only with respect to matrix and analyte concentration in the sample but also to concentrations and uncertainties of certified values in the CRM used. In the extreme trace analysis, CRMs with relatively large uncertainties and very low certified concentrations can still yield rather high information gain of results. (author) 14 refs.; 9 figs

Report of the consultants meeting on proper use of reference and control materials

International Nuclear Information System (INIS)

2002-01-01

Quality control in analytical laboratories as a basis of a complete quality system needs still to be developed in many Member States. To support the dissemination of information in this field a consultants meeting on 'Proper Use of Reference and Quality Control Materials' was held at the IAEA Headquarters, Vienna, from 13 to 17 August 2001. The experts convened with the objective to prepare a TECDOC to advise analytical laboratories in Member States on the correct use of Certified Reference Materials (CRMs) for Quality Control purposes and give practical recommendations to expand this concept to in-house Quality Control Materials (QCMs). In view of the existing literature in this field an urgent need for a practical guidebook for the preparation and application of cost effective and matrix matching QCMs was identified and the experts tried to fill this gap from their relevant experience. One and a half days of lecturing was followed by intensive discussion and brain storming to create a list of key words, which were structured in a logical order to provide a frame for the projected document. Responsibilities were assigned and deadlines fixed for the submission of the full text. (author)

Report of the consultants meeting on proper use of reference and control materials

Energy Technology Data Exchange (ETDEWEB)

NONE

2002-07-01

Quality control in analytical laboratories as a basis of a complete quality system needs still to be developed in many Member States. To support the dissemination of information in this field a consultants meeting on 'Proper Use of Reference and Quality Control Materials' was held at the IAEA Headquarters, Vienna, from 13 to 17 August 2001. The experts convened with the objective to prepare a TECDOC to advise analytical laboratories in Member States on the correct use of Certified Reference Materials (CRMs) for Quality Control purposes and give practical recommendations to expand this concept to in-house Quality Control Materials (QCMs). In view of the existing literature in this field an urgent need for a practical guidebook for the preparation and application of cost effective and matrix matching QCMs was identified and the experts tried to fill this gap from their relevant experience. One and a half days of lecturing was followed by intensive discussion and brain storming to create a list of key words, which were structured in a logical order to provide a frame for the projected document. Responsibilities were assigned and deadlines fixed for the submission of the full text. (author)

Critical Evaluation of an Intercalibration Project Focused on the Definition of New Multi-Element Soil Reference Materials (AMS-MO1 and AMS-ML1

Directory of Open Access Journals (Sweden)

Livia Vittori Antisari

2014-12-01

Full Text Available Soils are complex matrices and their geochemical investigation necessarily needs reliable Certified Reference Materials (CRMs, i.e. standards, to support analytical precision and accuracy. In particular, the definition of soil multi-element CRMs is particularly complex and involves an inter-laboratory program that employs numerous analytical techniques. In this study, we present the results of the inter-calibration experiment focused on the certification of two new soil standards named AMS-ML1 and AMS-MO1. The two soils developed on sandstone and serpentinite parent materials, respectively. The experiment involved numerous laboratories and focused on the evaluation of soil physicochemical parameters and geochemical analyses of major and trace elements by X-ray fluorescence (XRF and Inductive Coupled Plasma techniques (ICP-OES and ICP-MS. The data was statistically elaborated. Three levels of repeatability and accuracy in function of the different analytical methods and instrumentation equipment was observed. The statistical evaluation of the results obtained by ICP-OES on Aqua Regia extracts (i.e., Lilliefors test for normally, Grubbs test for outliers, Cochran test for outliers in variances and ANOVA allowed to computed some certified values for the two proposed soil standards. This preliminary study will represent the first step of a more thorough intercalibration ring-test involving a higher number of laboratories, in order to propose the investigated matrices as CRMs.

Development of a new ferulic acid certified reference material for use in clinical chemistry and pharmaceutical analysis

Directory of Open Access Journals (Sweden)

Dezhi Yang

2015-05-01

Full Text Available This study compares the results of three certified methods, namely differential scanning calorimetry (DSC, the mass balance (MB method and coulometric titrimetry (CT, in the purity assessment of ferulic acid certified reference material (CRM. Purity and expanded uncertainty as determined by the three methods were respectively 99.81%, 0.16%; 99.79%, 0.16%; and 99.81%, 0.26% with, in all cases, a coverage factor (k of 2 (P=95%. The purity results are consistent indicating that the combination of DSC, the MB method and CT provides a confident assessment of the purity of suitable CRMs like ferulic acid.

Development of a new ferulic acid certified reference material for use in clinical chemistry and pharmaceutical analysis.

Science.gov (United States)

Yang, Dezhi; Wang, Fengfeng; Zhang, Li; Gong, Ningbo; Lv, Yang

2015-05-01

This study compares the results of three certified methods, namely differential scanning calorimetry (DSC), the mass balance (MB) method and coulometric titrimetry (CT), in the purity assessment of ferulic acid certified reference material (CRM). Purity and expanded uncertainty as determined by the three methods were respectively 99.81%, 0.16%; 99.79%, 0.16%; and 99.81%, 0.26% with, in all cases, a coverage factor (k) of 2 (P=95%). The purity results are consistent indicating that the combination of DSC, the MB method and CT provides a confident assessment of the purity of suitable CRMs like ferulic acid.

Development of a reference material for routine performance monitoring of methods measuring polychlorinated dibenzo-p-dioxins, polychlorinated dibenzofurans and dioxin-like polychlorinated biphenyls.

Science.gov (United States)

Selliah, S S; Cussion, S; MacPherson, K A; Reiner, E J; Toner, D

2001-06-01

Matrix-matched environmental certified reference materials (CRMs) are one of the most useful tools to validate analytical methods, assess analytical laboratory performance and to assist in the resolution of data conflicts between laboratories. This paper describes the development of a lake sediment as a CRM for polychorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and dioxin-like polychlorinated biphenyls (DLPCBs). The presence of DLPCBs in the environment is of increased concern and analytical methods are being developed internationally for monitoring DLPCBs in the environment. This paper also reports the results of an international interlaboratory study involving thirty-five laboratories from seventeen countries, conducted to characterize and validate levels of a sediment reference material for PCDDs, PCDFs and DLPCBs.

Development of thoria certified reference materials-role of NFC

International Nuclear Information System (INIS)

Balaji Rao, Y.; Yadav, R.B.; Ramana Rao, A.V.

2007-01-01

The present paper discusses the different phases of Inter Laboratory Comparison Experiments (ILCE) program for development of thoria CRMs with a special emphasis on the role played by Control Laboratory, NFC. The preparation of ThO 2 CRMs along with their importance in analysis is also explained in the paper. (author)

Use of CRM's as mutual calibrating materials and control of synthetic multielement standards as used in INAA

International Nuclear Information System (INIS)

Rossbach, M.; Stoeppler, M.

1987-01-01

Dilution effects of different multielement synthetic standard solutions were studied by measuring 10-12 different concentrations of the same solution. Peak area comparison of four Certified Reference Materials (CRMs) using one value for the evaluation of the other three repetitively led to the intercomparison (degree of compatibility) of the certified values. The idea of the preparation of each laboratory's 'secondary reference standard' by comparison of synthetic multielement standards with as many CRMs as practically feasible is advocated to improve the reliability of analytical results. (author)

Determination of rare earth and uranium in reference biological materials certified by the method of neutron activation analysis; Determinacao de terras raras e de uranio em materiais biologicos de referencia certificados pelo metodo de analise por ativacao com neutrons

Energy Technology Data Exchange (ETDEWEB)

Pereira, Lais H.P.; Saiki, Mitiko, E-mail: laispaciulli@gmail.com, E-mail: mitiko@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

2013-07-01

The objective of this study was to evaluate the precision and accuracy of the determinations of Sc, La, Ce, Nd, Sm, Eu, Tb, Yb, Lu and U in certified reference materials (CRMs). To solve the problem of interference from fission products of U in the determination of lanthanides were obtained correction factors for this interference for {sup 140}La, {sup 141}Ce, {sup 143}Ce, {sup 153}Sm and {sup 147}Nd. The experimental procedure of Neutron Activation Analysis consisted of irradiating aliquots of each of the CRMs with synthetic standards of elements under thermal neutron flux of the IEA-R1 nuclear reactor, followed by gamma-ray spectrometry using a high-resolution hyperpurity GE detector. The analyzes of CRMs indicate good accuracy and precision of results, demonstrating the feasibility of applying of established procedure in NAA of elements studied in organic vegetable matrices.

The use of reference materials in quality assurance programmes in food microbiology laboratories.

Science.gov (United States)

In't Veld, P H

1998-11-24

Nine different reference materials (RMs) for use in food and water microbiology have been developed with the support of the European Commission (EC). The production process of RMs is based on spray drying bacteria suspended in milk. The highly contaminated milk powder (HCMP) obtained is mixed with sterile milk powder to achieve the desired level of contamination and is subsequently filled into gelatine capsules. The HCMP may need to be stabilised by storage for more than a year before a stable RM can be prepared. The HCMP are mixed with sterile milk powder using a pestle and mortar in order to produce homogeneous RMs. For routine use of RMs Shewhart control charts can be produced. Based on log10 transformed counts, control limits are calculated. Rules for the interpretation of results facilitate the detection of out of control situations. Besides RMs there are also CRMs (Certified Reference Materials) that are certified by the EC Community Bureau of Reference (BCR) and are intended for occasional use. Based on the BCR certificate, user tables are produced presenting the 95% confidence limits for the number of capsules likely to be examined in practice. Also power analysis is made to indicate the minimum difference between the certified value and the observed geometric mean value in relation to the number of capsules examined.

A Development Strategy for Creating a Suite of Reference Materials for the in-situ Microanalysis of Non-conventional Raw Materials

Science.gov (United States)

Renno, A. D.; Merchel, S.; Michalak, P. P.; Munnik, F.; Wiedenbeck, M.

2010-12-01

Recent economic trends regarding the supply of rare metals readily justify scientific research into non-conventional raw materials, where a particular need is a better understanding of the relationship between mineralogy, microstructure and the distribution of key metals within ore deposits (geometallurgy). Achieving these goals will require an extensive usage of in-situ microanalytical techniques capable of spatially resolving material heterogeneities which can be key for understanding better resource utilization. The availability of certified reference materials (CRMs) is an essential prerequisite for (1) validating new analytical methods, (2) demonstrating data quality to the contracting authorities, (3) supporting method development and instrument calibration, and (4) establishing traceability between new analytical approaches and existing data sets. This need has led to the granting of funding by the European Union and the German Free State of Saxony for a program to develop such reference materials . This effort will apply the following strategies during the selection of the phases: (1) will use exclusively synthetic minerals, thereby providing large volumes of homogeneous starting material. (2) will focus on matrices which are capable of incorporating many ‘important’ elements while avoid exotic compositions which would not be optimal matrix matches. (3) will emphasise those phases which remain stable during the various microanalytical procedure. This initiative will assess the homogeneity of the reference materials at sampling sizes ranging between 50 and 1 µm; it is also intended to document crystal structural homogeneity too, as this too may potentially impact specific analytical methods. As far as possible both definitive methods as well as methods involving matrix corrections will be used for determining the compositions of the of the individual materials. A critical challenge will be the validation of the determination of analytes concentrations

Recent applications of nuclear analytical methods to the certification of elemental content in NIST standard reference materials

International Nuclear Information System (INIS)

Greenberg, R.R.; Zeisler, R.; Mackey, E.A.

2006-01-01

Well-characterized, certified reference materials (CRMs) play an essential role in assuring the quality of analytical measurements. NIST has been producing CRMs, currently called NIST Standard Reference Materials (SRMs), to validate analytical measurements for nearly one hundred years. The predominant mode of certifying inorganic constituents in complex-matrix SRMs is through the use of two critically evaluated, independent analytical techniques at NIST. These techniques should have no significant sources of error in common. The use of nuclear analytical methods in combination with one of the chemically based analytical method at NIST eliminates the possibility of any significant, common error source. The inherent characteristics of the various forms of nuclear analytical methods make them extremely valuable for SRM certification. Instrumental NAA is nondestructive, which eliminates the possibility of any dissolution problems, and often provides homogeneity information. Radiochemical NAA typically provides nearly blank-free determinations of some highly important, but difficult elements at very low levels. Prompt-gamma NAA complements INAA, and provides independent determinations of some key elements. In addition, all significant uncertainty components can be evaluated for these techniques, and we believe these methods can meet all the requirements of a primary method of measurement as defined by ISO and the CCQM. NIST has certified several SRMs using INAA and RNAA as primary methods. In addition, NIST has compared measurements by INAA and PGAA with other primary methods as part of the CCQM intercomparisons of national metrology institutes. Some significant SRMs recently certified for inorganic constituents with contributions from the nuclear analytical methods include: Toxic Substances in Urine (SRM 2670a), Lake Superior Fish Tissue (SRM 1946), Air Particulate on Filter Media (SRM 2783), Inorganics in Marine Sediment (SRM 2702), Sediment for Solid Sampling (Small

Development of certified matrix-based reference material of genetically modified rice event TT51-1 for real-time PCR quantification.

Science.gov (United States)

Jiang, Yu; Yang, Hui; Quan, Sheng; Liu, Yinan; Shen, Ping; Yang, Litao

2015-09-01

In 2009, the genetically modified (GM) rice event TT51-1 with an engineered insect resistance trait became the first GM rice event to be granted certification for safe production in China, and its derivative lines Bt 63 and Huahui No.1 are expected to be commercialized soon. The development of certified reference material (CRM) for TT51-1 is necessary to monitor and inspect the TT51-1 event and its derivates. In this work, we developed four matrix-based TT51-1 rice CRMs (TT51-1a, TT51-1b, TT51-1c, and TT51-1d) with different TT51-1 mass fraction ratios by blending seed powders of homozygous TT51-1 and its recipient cultivar Minghui 63. The between-bottle homogeneity and the within-bottle homogeneity were tested, and good results were obtained. The potential degradation during transportation and shelf life were evaluated, and demonstrated an expiration period of at least 36 months. The characterization values of the four TT51-1 CRMs based on the mass fraction ratio were 1000.000 ± 51.430 g/kg, 49.940 ± 4.620 g/kg, 9.990 ± 1.110 g/kg, and 4.990 ± 0.620 g/kg, respectively. The characterization values based on the copy number ratio were certified by digital PCR analysis as 97.442 ± 5.253 %, 4.851 ± 0.486 %, 1.042 ± 0.135 %, and 0.556 ± 0.073 %, respectively. These results suggested that the TT51-1 matrix-based CRMs developed are of high quality and can be used as potential calibrators for TT51-1 GM rice inspection and monitoring.

Uranium reference materials

International Nuclear Information System (INIS)

Donivan, S.; Chessmore, R.

1987-07-01

The Technical Measurements Center has prepared uranium mill tailings reference materials for use by remedial action contractors and cognizant federal and state agencies. Four materials were prepared with varying concentrations of radionuclides, using three tailings materials and a river-bottom soil diluent. All materials were ground, dried, and blended thoroughly to ensure homogeneity. The analyses on which the recommended values for nuclides in the reference materials are based were performed, using independent methods, by the UNC Geotech (UNC) Chemistry Laboratory, Grand Junction, Colorado, and by C.W. Sill (Sill), Idaho National Engineering Laboratory, Idaho Falls, Idaho. Several statistical tests were performed on the analytical data to characterize the reference materials. Results of these tests reveal that the four reference materials are homogeneous and that no large systematic bias exists between the analytical methods used by Sill and those used by TMC. The average values for radionuclides of the two data sets, representing an unbiased estimate, were used as the recommended values for concentrations of nuclides in the reference materials. The recommended concentrations of radionuclides in the four reference materials are provided. Use of these reference materials will aid in providing uniform standardization among measurements made by remedial action contractors. 11 refs., 9 tabs

Specifications for trueness and precision of a reference measurement system for serum/plasma 25-hydroxyvitamin D analysis.

Science.gov (United States)

Stöckl, Dietmar; Sluss, Patrick M; Thienpont, Linda M

2009-10-01

The divergence in analytical quality of serum/plasma 25-hydroxy-vitamin D analysis calls for defining specifications for a reference measurement system. Fundamentally, in a reference measurement system, there should be a relationship between the analytical specifications for higher- (reference) and lower-order (routine) measurements. Therefore, when setting specifications, we started with limits for routine imprecision (CV(rou)) and bias (B(rou)) using 4 models: (1) the misclassifications in diagnosis, (2) biological variation data (reference interval (RI) and monitoring), (3) expert recommendations, and (4) state-of-the-art performance. Then, we used the derived goals to tailor those for reference measurements and certified reference materials (CRMs) for calibration by setting the limits for CV(ref) at 0.5 CV(rou), B(ref) at 0.33 B(rou)(,) max. uncertainty (U(max)) at 0.33 B(ref). The established specifications ranged between CV(rou)model 3) and CV(rou)model 2, monitoring). Model 2 (monitoring) gave the most stringent goals, model 3, the most liberal ones. Accounting for state-of-the-art performance and certification capabilities, we used model 2 (RI) to recommend achievable goals: for routine testing, CV(rou)measurements, CV(ref)CRMs, U(max) 0.6%.

Intercomparison and certification of some Chinese and international food and biological matrix CRMs for several uncertified ultratrace elements by NAA

International Nuclear Information System (INIS)

Weizhi, T.; Bangfa, N.; Pingsheng, W.; Huiling, N.; Lei, C.; Yangmei, Z.

2001-01-01

Radiochemical neutron activation analysis was used for determinations of 8 rare elements (La, Ce, Nd, Sm, Eu, Tb, Yb and Lu) in two Chinese CRMs, GBW 08503 (wheat) and GBW 09101 (hair), and Cs, Sr, Th and U in five NIST SRMs, 1548 (Total Diet), 1486 (Bone Meal), 8414 (Bovine Muscle), 1566a (Oyster Powder ) and 1575 (Pine Needles). These determinations are for eventual certification of above ultratrace elements so far not certified. The radiochemical separation scheme used in RNAA of NIST SRMs is an anion exchange followed by the coprecipitation by (REE)F 3 for U and Th, and SrSo 4 precipitation for Sr and Cs. For RNAA of the two Chinese CRMs, a one step (REE)F 3 precipitation was used. Chemical yields were determined for all relevant elements by tracer experiments. All these materials were also analyzed by ICPMS, that offered an opportunity to compare the two major trace analytical techniques on their merits and drawbacks for these particular cases. RNAA is proven to be one of the important techniques in ultratrace analysis, especially in certification of some ultratrace elements. Determination of elements in sub-ng/g level is still an area to be further investigated because: (1) some such elements are important in food and health related environmental studies, (2) many of these elements have no (or very few) certified values in existing biological CRMs, (3) reliable techniques qualified for ultratrace analysis are needed to be established, and (4) sampling behavior of elements at these levels is still not very well known (recommended minimum sample size may not be adequate). (author)

IAEA biological reference materials

International Nuclear Information System (INIS)

Parr, R.M.; Schelenz, R.; Ballestra, S.

1988-01-01

The Analytical Quality Control Services programme of the IAEA encompasses a wide variety of intercomparisons and reference materials. This paper reviews only those aspects of the subject having to do with biological reference materials. The 1988 programme foresees 13 new intercomparison exercises, one for major, minor and trace elements, five for radionuclides, and seven for stable isotopes. Twenty-two natural matrix biological reference materials are available: twelve for major, minor and trace elements, six for radionuclides, and four for chlorinated hydrocarbons. Seven new intercomparisons and reference materials are in preparation or under active consideration. Guidelines on the correct use of reference materials are being prepared for publication in 1989 in consultation with other major international producers and users of biological reference materials. The IAEA database on available reference materials is being updated and expanded in scope, and a new publication is planned for 1989. (orig.)

New Polish Certified Reference Materials for inorganic trace analysis: corn flour (INCT-CF-3) and soya bean flour (INCT-SBF-4)

International Nuclear Information System (INIS)

Polkowska-Motrenko, H.; Dybczynski, R.S.; Chajduk, E.; Danko, B.; Kulisa, K.; Samczynski, Z.; Sypula, M.; Szopa, Z.

2007-01-01

Preparation and certification of two new Polish reference materials (CRMs) for inorganic trace analysis: Corn Flour (INCT-CF-3) and Soya Bean Flour (INCT-SBF-4) have been presented. The materials were prepared and certified in the Institute of Nuclear Chemistry and Technology, Warsaw (INCT). Instrumental neutron activation analysis (INAA) was applied to homogeneity and stability studies. Homogeneity tests have shown that both materials are homogeneous for the sample mass 3 100 mg. The results of trend analysis have shown that the materials are stable. Uncertainty caused by instability and, consequently, shelf life of the materials have been estimated. Certification was based on the statistical evaluation of results obtained in worldwide interlaboratory comparison, in which 92 laboratories from 19 countries participated. Results for CRM distributed by the organizer and analyzed together with the intercomparison samples as well as results by definitive methods for selected elements based on radiochemical neutron activation analysis (RNAA) were also employed in the certification process. The contents of 16 and 22 elements were certified in Corn Flour and Soya Bean Flour, respectively. Additional information values for 14 elements in INCT-CF-3 and 9 elements in INCT-SBF-4 were given. (authors)

Experience of air transport of nuclear fuel material in Japan

International Nuclear Information System (INIS)

Yamashita, T.; Toguri, D.; Kawasaki, M.

2004-01-01

Certified Reference Materials (hereafter called as to CRMs), which are indispensable for Quality Assurance and Material Accountability in nuclear fuel plants, are being provided by overseas suppliers to Japanese nuclear entities as Type A package (non-fissile) through air transport. However, after the criticality accident at JCO in Japan, special law defining nuclear disaster countermeasures (hereafter called as to the LAW) has been newly enforced in June 2000. Thereafter, nuclear fuel materials must meet not only to the existing transport regulations but also to the LAW for its transport

Micro-homogeneity of candidate reference materials: Results from an intercomparison study for the Analytical Quality Control Services (AQCS) of the IAEA

International Nuclear Information System (INIS)

Rossbach, M.; Kniewald, G.

2002-01-01

The IAEA Analytical Quality Control Services (AQCS) has made available two single cell algae materials IAEA-392 and IAEA-393 as well as an urban dust IAEA-396 to study their use for analytical sample sizes in the milligram range and below. Micro-analytical techniques such as PIXE and μ-PIXE, solid sampling AAS, scanning electron microprobe X-ray analysis and INAA were applied to the determination of trace elements on the basis of μg to mg amounts of the selected materials. The comparability of the mean values as well as the reproducibility of successive measurements is being evaluated in order to compare relative homogeneity factors for many elements in the investigated materials. From the reported results it seems that the algae materials IAEA-392 and IAEA-393 are extremely homogeneous biological materials for a number of elements with an extraordinary sharp particle size distribution below 10 μm. A similar situation seems to hold for the urban dust material IAEA-396 which had been air-jet milled to a particle size distribution around 4 μm. The introduction of these materials as CRMs with very small amounts needed to determine the certified concentrations will help to meet the needs of micro-analytical techniques for natural matrix reference materials. (author)

Single-particle characterization of 'Asian Dust' certified reference materials using low-Z particle electron probe X-ray microanalysis

International Nuclear Information System (INIS)

Hwang, Hee Jin; Ro, Chul-Un

2006-01-01

In order to clearly elucidate whether Asian Dust particles experience chemical modification during long-range transport, it is necessary to characterize soil particles where Asian Dust particles originate. If chemical compositions of source soil particles are well characterized, then chemical compositions of Asian Dust particles collected outside source regions can be compared with those of source soil particles in order to find out the occurrence of chemical modification. Asian Dust particles are chemically and morphologically heterogeneous, and thus the average composition and the average aerodynamic diameter (obtainable by bulk analysis) are not much relevant if the chemical modifications of the particles must be followed. The major elemental composition and abundance of the particle types that are potential subjects of chemical modification can only be obtained using single-particle analysis. A single particle analytical technique, named low-Z particle electron probe X-ray microanalysis (low-Z particle EPMA), was applied to characterize two certified reference materials (CRMs) for Asian Dust particles, which were collected from a loess plateau area and a desert of China. The CRMs were defined by bulk analyses to provide certified concentrations for 13 chemical elements. Using the low-Z particle EPMA technique, the concentrations of major chemical species such as aluminosilicates, SiO 2 , CaCO 3 , and carbonaceous species were obtained. Elemental concentrations obtained by the low-Z particle EPMA are close to the certified values, with considering that the single particle and bulk analyses employ very different approaches. There are still some discrepancies between those concentration values, resulting from analyses of particles with different sizes, different sample amounts analyzed, and uncertainties involved in the single particle analysis

Development of a highly precise ID-ICP-SFMS method for analysis of low concentrations of lead in rice flour reference materials.

Science.gov (United States)

Zhu, Yanbei; Inagaki, Kazumi; Yarita, Takashi; Chiba, Koichi

2008-07-01

Microwave digestion and isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-SFMS) has been applied to the determination of Pb in rice flour. In order to achieve highly precise determination of low concentrations of Pb, the digestion blank for Pb was reduced to 0.21 ng g(-1) after optimization of the digestion conditions, in which 20 mL analysis solution was obtained after digestion of 0.5 g rice flour. The observed value of Pb in a non-fat milk powder certified reference material (CRM), NIST SRM 1549, was 16.8 +/- 0.8 ng g(-1) (mean +/- expanded uncertainty, k = 2; n = 5), which agreed with the certified value of 19 +/- 3 ng g(-1) and indicated the effectiveness of the method. Analytical results for Pb in three brown rice flour CRMs, NIST SRM 1568a, NIES CRM 10-a, and NIES CRM 10-b, were 7.32 +/- 0.24 ng g(-1) (n = 5), 1010 +/- 10 ng g(-1) (n = 5), and 1250 +/- 20 ng g(-1) (n = 5), respectively. The concentration of Pb in a candidate white rice flour reference material (RM) sample prepared by the National Metrology Institute of Japan (NMIJ) was observed to be 4.36 +/- 0.28 ng g(-1) (n = 10 bottles).

Survey of reference materials. V. 2: Environmentally related reference materials for trace elements, nuclides and microcontaminants

International Nuclear Information System (INIS)

1996-05-01

The present report presently contains over 250 reference materials with trace element and organic contaminant information on fuel, geological and mineral, anthropogenic disposal, soil reference and miscellaneous reference materials. Not included in the current report is information on most biological and environmental reference materials with trace element, stable isotope, radioisotope and organic contaminant information. 8 refs, tabs

Reference materials and representative test materials: the nanotechnology case

International Nuclear Information System (INIS)

Roebben, G.; Rasmussen, K.; Kestens, V.; Linsinger, T. P. J.; Rauscher, H.; Emons, H.; Stamm, H.

2013-01-01

An increasing number of chemical, physical and biological tests are performed on manufactured nanomaterials for scientific and regulatory purposes. Existing test guidelines and measurement methods are not always directly applicable to or relevant for nanomaterials. Therefore, it is necessary to verify the use of the existing methods with nanomaterials, thereby identifying where modifications are needed, and where new methods need to be developed and validated. Efforts for verification, development and validation of methods as well as quality assurance of (routine) test results significantly benefit from the availability of suitable test and reference materials. This paper provides an overview of the existing types of reference materials and introduces a new class of test materials for which the term ‘representative test material’ is proposed. The three generic concepts of certified reference material, reference material(non-certified) and representative test material constitute a comprehensive system of benchmarks that can be used by all measurement and testing communities, regardless of their specific discipline. This paper illustrates this system with examples from the field of nanomaterials, including reference materials and representative test materials developed at the European Commission’s Joint Research Centre, in particular at the Institute for Reference Materials and Measurements (IRMM), and at the Institute for Health and Consumer Protection (IHCP).

Nuclear measurements and reference materials

International Nuclear Information System (INIS)

1988-01-01

This report summarizes the progress of the JRC programs on nuclear data, nuclear metrology, nuclear reference materials and non-nuclear reference materials. Budget restrictions and personnel difficulties were encountered during 1987. Fission properties of 235 U as a function of neutron energy and of the resonances can be successfully described on the basis of a three exit channel fission model. Double differential neutron emission cross-sections were accomplished on 7 Li and were started for the tritium production cross-section of 9 Be. Reference materials of uranium minerals and ores were prepared. Special nuclear targets were prepared. A batch of 250 g of Pu0 2 was characterized in view of certification as reference material for the elemental assay of plutonium

COMAR - database for certified reference materials

International Nuclear Information System (INIS)

Klich, H.; Caliste, J.P.

1988-01-01

With more than 130 producers of reference materials (RM) throughout the world, it is often difficult to find the best reference material for a specific application. The computer database COMAR has been developed to aid chemists in finding the needed reference material. (orig.)

Reference materials: recent developments in health, food safety and environmental areas

International Nuclear Information System (INIS)

Iyengar, V.; Gills, T.E.

1998-01-01

In the 1980s, CRMs were gradually recognized as an integral part of analytical chemistry as effective tools to verify accuracy of methods. Subsequently, new technologies emerged, and these were capable of processing complex materials without compromising matrix integrity and analyte stability over extended periods of storage. The sequence of events can be outlined as follows: (1) improvements in inorganic methods of analysis, where nuclear analytical techniques played a crucial role, (2) identification of RM needs and assays for organic constituents in foods and environmental materials, (3) a clear understanding of the distinction between primary (certified) and secondary (e.g. check samples for proficiency testing) types of RMs, (4) preparing specific RMs (spiked standards) to address matrix related measurement problems, (5) preparation of slurry and composite (freeze dried and frozen) types of RMs, (6) realization of the need for a global vision in dealing with standards as illustrated by the activities of GESREM, (7) concern for traceability of chemical measurements to internationally recognized standards, and (8) recognition of the need for multidisciplinary approaches for preparing certain types of RMs (e.g. microbiological RMs) in response to the regulatory measurement needs of food safety and environmental health criteria

A routine chromium determination in biological materials; application to various reference materials and standard reference materials

International Nuclear Information System (INIS)

Tjioe, P.S.; Goeij, J.J.M. de; Volkers, K.J.

1979-01-01

The determination limit under standard working conditions of chromium in biological materials is discussed. Neutron activation analysis and atomic spectrometry have been described for some analytical experiences with NBS SRM 1577 reference material. The chromium determination is a part of a larger multi-element scheme for the determination of 12 elements in biological materials

Preparation of plant-specific NDA reference material

International Nuclear Information System (INIS)

Abedin-Zadeh, R.; Beetle, T.; Kuhn, E.; Terrey, D.; Turel, S.; Busca, G.; Guardini, S.

1983-01-01

The importance of having suitable and well characterized non-destructive assay (NDA) reference materials for the verification activities of the safeguards control authorities is stressed. The Euratom Inspectorate and the IAEA have initiated an extensive programme for the procurement and preparation of Joint Euratom/IAEA safeguards NDA reference materials with the active participation of the Ispra Establishment of the Euratom Joint Research Centre. The different type and nature of materials, condition of measurements, and plant characteristics and provisions had to be taken into account for plant-specific NDA reference materials. The preparation of each reference material was planned case by case and specific criteria such as limitations in different facilities, measurement capabilities, conditions, product availability and population variability are being ascertained. A procurement scheme was prepared describing step-by-step procedures detailing responsibilities, measurement conditions, destructive analysis schemes, desired characteristics and methods of data evaluation. This paper describes the principles and procedures carried out for the preparation of a reference MOX pin, low enriched uranium reference rods, low enriched uranium reference drums, reference MTR assemblies, and THTR reference pebbles. The scheme for each characterization technique is presented. (author)

NBS activities in biological reference materials

Energy Technology Data Exchange (ETDEWEB)

Rasberry, S.D.

1988-12-01

NBS activities in biological reference materials during 1986-1988 are described with a preview of plans for future certifications of reference materials. During the period, work has been completed or partially completed on about 40 reference materials of importance to health, nutrition, and environmental quality. Some of the reference materials that have been completed during the period and are described include: creatinine (SRM 914a), bovine serum albumin (SRM 927a), cholesterol in human serum (SRM's 1951-1952), aspartate aminotransferase (RM 8430), cholesterol and fat-soluble vitamins in coconut oil (SRM 1563), wheat flour (SRM 1567a), rice flour (SRM 1568a), mixed diet (RM 8431a), dinitropyrene isomers and 1-nitropyrene (SRM 1596), and complex PAH's from coal tar (SRM 1597). Oyster tissue (SRM 1566a) is being analyzed and should be available in 1988.

Reference material systems: a sourcebook for material assessment

Energy Technology Data Exchange (ETDEWEB)

Bhagat, N. (ed.)

1976-12-01

A reference set of data related to material systems and a framework for carrying out the material technologies assessment are presented. While the bulk of renewables have been considered in this report, the nonrenewable materials dealt with here include structural materials only, such as steel, aluminum, cement and concrete, and bricks. The complete data set is supposed to include material flows, energy requirements, capital and labor inputs, and environmental effects for each process that a resource must go through to become a useful material for an end use. Although effort has been made to obtain as much information as possible, considerable gaps in data, apparent throughout this report, could not be avoided. A new material technology can be evaluated by substituting that technology for appropriate elements of the reference materials system and calculating the net change in material resource, energy, capital and labor requirements, and environmental impacts. This combination of information thus serves as a means of evaluating the potential benefits to be gained by research in various material technologies.

15 CFR 230.3 - New Standard Reference Materials.

Science.gov (United States)

2010-01-01

... NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY, DEPARTMENT OF COMMERCE STANDARD REFERENCE MATERIALS STANDARD REFERENCE MATERIALS General Information § 230.3 New Standard Reference Materials. When new SRM's... scientific and trade journals. ...

Value assignment of nutrient concentrations in five standard reference materials and six reference materials.

Science.gov (United States)

Sharpless, K E; Gill, L M

2000-01-01

A number of food-matrix reference materials (RMs) are available from the National Institute of Standards and Technology (NIST) and from Agriculture Canada through NIST. Most of these materials were originally value-assigned for their elemental composition (major, minor, and trace elements), but no additional nutritional information was provided. Two of the materials were certified for selected organic constituents. Ten of these materials (Standard Reference Material [SRM] 1,563 Cholesterol and Fat-Soluble Vitamins in Coconut Oil [Natural and Fortified], SRM 1,566b Oyster Tissue, SRM 1,570a Spinach Leaves, SRM 1,974a Organics in Mussel Tissue (Mytilus edulis), RM 8,415 Whole Egg Powder, RM 8,418 Wheat Gluten, RM 8,432 Corn Starch, RM 8,433 Corn Bran, RM 8,435 Whole Milk Powder, and RM 8,436 Durum Wheat Flour) were recently distributed by NIST to 4 laboratories with expertise in food analysis for the measurement of proximates (solids, fat, protein, etc.), calories, and total dietary fiber, as appropriate. SRM 1846 Infant Formula was distributed as a quality control sample for the proximates and for analysis for individual fatty acids. Two of the materials (Whole Egg Powder and Whole Milk Powder) were distributed in an earlier interlaboratory comparison exercise in which they were analyzed for several vitamins. Value assignment of analyte concentrations in these 11 SRMs and RMs, based on analyses by the collaborating laboratories, is described in this paper. These materials are intended primarily for validation of analytical methods for the measurement of nutrients in foods of similar composition (based on AOAC INTERNATIONAL's fat-protein-carbohydrate triangle). They may also be used as "primary control materials" in the value assignment of in-house control materials of similar composition. The addition of proximate information for 10 existing reference materials means that RMs are now available from NIST with assigned values for proximates in 6 of the 9 sectors of

The role of certified reference materials in material control and accounting

International Nuclear Information System (INIS)

Turel, S.P.

1979-01-01

One way of providing an adequate material control and accounting system for the nuclear fuel cycle is to calculate material unaccounted for (MUF) after a physical inventory and to compare the limit of error of the MUF value (LEMUF) against prescribed criteria. To achieve a meaningful LEMUF, a programme for the continuing determination of systematic and random errors is necessary. Within this programme it is necessary to achieve traceability of all Special Nuclear Material (SNM) control and accounting measurements to an International/National Measurement System by means of Certified Reference Materials. SNM measurements for control and accounting are made internationally on a great variety of materials using many diverse measurement procedures by a large number of facilities. To achieve valid overall accountability over this great variety of measurements there must be some means of relating all these measurements and their uncertainties to each other. This is best achieved by an International/National Measurement System (IMS/NMS). To this end, all individual measurement systems must be compatible to the IMS/NMS and all measurement results must be traceable to appropriate international/national Primary Certified Reference Materials. To obtain this necessary compatibility for any given SNM measurement system, secondary certified reference materials or working reference materials are needed for every class of SNM and each type of measurement system. Ways to achieve ''traceability'' and the various types of certified reference material are defined and discussed in this paper. (author)

AQCS 1989 - Intercomparison runs reference materials

International Nuclear Information System (INIS)

1989-01-01

The purpose of the Analytical Quality Control Services (AQCS) programme provided by the International Atomic Energy Agency (Agency) is to assist laboratories engaged in the analysis of nuclear, environmental, biological, and materials of marine origin for radionuclide, major, minor and trace elements, as well as stable isotopes using atomic and nuclear analytical techniques, to check the quality of their work. Reference Materials available are listed by origin and by analyte giving referenced values and confidence intervals. Only materials, which have one or more properties sufficiently well established from statistical evaluation of previous interlaboratory comparison studies are included. Existing Reference Materials may be updated for previously referenced constituents or properties according to the results of the Agency's Co-ordinated Research Programmes (CRPs) in these fields or according to recently published literature values. They are supplied with a reference sheet stating relevant parameters and properties of the material and can be used as secondary standards for quality control assurance within a laboratory, for checking analytical methods and/or instrumentation or for training purposes. 4 tabs

235Uranium isotope abundance certified reference material for gamma spectrometry EC nuclear reference material 171 certification report

International Nuclear Information System (INIS)

De Bievre, P.; Eschbach, H.L.; Lesser, R.; Meyer, H.; Audenhove, Van J.

1986-01-01

This certification report contains the information necessary for the final certification of EC nuclear reference material 171. It is also intended to inform the user of the reference material concerned on technical/scientific details which are not given in the certificate. The report describes the reference material which consists of sets of U 3 O 8 samples with five different 235 U/U abundances, filled in cylindrical aluminium cans. The can bottom serves as window for emitted gamma radiation. The report describes how the 235 U/U abundances were characterized, how the other properties relevant for gamma measurements were determined and gives all connected results as well as those from the verification measurements. Appendix A represents the draft certificate. 32 refs

Reference materials for microanalytical nuclear techniques

Energy Technology Data Exchange (ETDEWEB)

Injuk, Jasna; Grieken, Rene van [Department of Chemistry, Micro and Trace Analysis Centre, University of Antwerp, Wilrijk-Antwerp (Belgium)

1994-07-01

This paper discusses some issues concerning reference materials required for microanalysis including physical and chemical properties of the sample matrix and homogeneity of the chemical composition. It gives some examples of the mst common standards used. Further the paper gives background information about the Micro- and Trace Analysis Center of the University of Antwerp, Belgium and discusses recent results of the Center in microanalysis of reference materials.

Computational exploration of cis-regulatory modules in rhythmic expression data using the "Exploration of Distinctive CREs and CRMs" (EDCC) and "CRM Network Generator" (CNG) programs.

Science.gov (United States)

Bekiaris, Pavlos Stephanos; Tekath, Tobias; Staiger, Dorothee; Danisman, Selahattin

2018-01-01

Understanding the effect of cis-regulatory elements (CRE) and clusters of CREs, which are called cis-regulatory modules (CRM), in eukaryotic gene expression is a challenge of computational biology. We developed two programs that allow simple, fast and reliable analysis of candidate CREs and CRMs that may affect specific gene expression and that determine positional features between individual CREs within a CRM. The first program, "Exploration of Distinctive CREs and CRMs" (EDCC), correlates candidate CREs and CRMs with specific gene expression patterns. For pairs of CREs, EDCC also determines positional preferences of the single CREs in relation to each other and to the transcriptional start site. The second program, "CRM Network Generator" (CNG), prioritizes these positional preferences using a neural network and thus allows unbiased rating of the positional preferences that were determined by EDCC. We tested these programs with data from a microarray study of circadian gene expression in Arabidopsis thaliana. Analyzing more than 1.5 million pairwise CRE combinations, we found 22 candidate combinations, of which several contained known clock promoter elements together with elements that had not been identified as relevant to circadian gene expression before. CNG analysis further identified positional preferences of these CRE pairs, hinting at positional information that may be relevant for circadian gene expression. Future wet lab experiments will have to determine which of these combinations confer daytime specific circadian gene expression.

On the development of quality assurance

DEFF Research Database (Denmark)

Andersen, Jens

2014-01-01

Contemporary research in quality assurance indicates that large uncertainties observed in interlaboratory comparisons to a large extent originate from a lack of competence of laboratory staff. This explanation is challenged by the present article for which six technologies and multiple series of ...... of uncertainties of certified reference materials (CRMs) gave results that differed significantly from those in the certificates of the CRMs. (C) 2014 Elsevier B.V. All rights reserved....

AQCS 1990. Intercomparison runs, reference materials

International Nuclear Information System (INIS)

1990-01-01

The purpose of the Analytical Quality Control Services (AQCS) programme provided by the International Atomic Energy Agency (Agency) is to assist laboratories engaged in the analysis of nuclear, environmental, biological, and materials of marine origin for radionuclide, major, minor and trace elements, as well as stable isotopes using atomic and nuclear analytical techniques, to check the quality of their work. Such a control is necessary since results of analytical activities may be the basis upon which economic, administrative, medical or legal decisions are taken; they must, therefore, be documented to be sufficiently reliable. The Agency has instituted the AQCS-programme which for 1990 will involve distributing samples for Intercomparison Runs and Reference Materials in a way similar to that of previous years. The Agency's Analytical Quality Control Services (AQCS) programme provides mainly three types of materials: materials which can be used in analytical laboratories working in the fields of nuclear technology and isotope hydrology. These include uranium ore Reference Materials and other substances of interest for nuclear fuel technology as well as stable isotope Reference Materials for mass spectrometric determination of isotope ratios in natural waters; materials with known content of uranium, thorium and/or transuranium elements or fission products for the determination of environmental radioactivity or control of nuclear safety; materials for use in the determination of stable trace elements in environmental, biomedical and marine research. Radiochemical methods such as neutron activation or isotope dilution analysis are often used in the determination of such trace elements and constitute an important contribution of nuclear techniques to applied science. Tabs

Development of solid water-equivalent radioactive certified reference materials

International Nuclear Information System (INIS)

Finke, E.; Greupner, H.; Groche, K.; Rittwag, R.; Geske, G.

1991-01-01

This paper presents a brief description of the development of solid water-equivalent beta volume radioactive certified reference materials. These certified reference materials were prepared for the beta fission nuclides 90 Sr/ 90 Y, 137 Cs, 147 Pm and 204 Tl. Comparative measurements of liquid and solid water-equivalent beta volume radioactive certified reference materials are discussed. (author)

New reference materials improvement of methods of measurements

International Nuclear Information System (INIS)

Marchandise, H.

1985-01-01

The report summarizes the development of about 120 reference materials in a variety of fields (non ferrous metals, trace element analysis, food products, biomedical analysis, physical and technical properties of solid materials). The document also provides practical advice for trace element analyses, describes the principles followed for certifying reference materials and provides recommendations for their use

Development of solid water-equivalent radioactive certified reference materials

Energy Technology Data Exchange (ETDEWEB)

Finke, E.; Greupner, H.; Groche, K.; Rittwag, R. (Office for Standardization, Metrology and Quality Control (ASMW), Berlin (Germany, F.R.)); Geske, G. (Jena Univ. (Germany, F.R.))

1991-01-01

This paper presents a brief description of the development of solid water-equivalent beta volume radioactive certified reference materials. These certified reference materials were prepared for the beta fission nuclides {sup 90}Sr/{sup 90}Y, {sup 137}Cs, {sup 147}Pm and {sup 204}Tl. Comparative measurements of liquid and solid water-equivalent beta volume radioactive certified reference materials are discussed. (author).

Nuclear forensics-metrological basis for legal defensibility

International Nuclear Information System (INIS)

Leggitt, J.; Inn, K.; Goldberg, S.; Essex, R.; LaMont, S.; Chase, S.

2009-01-01

The admissibility of nuclear forensics measurements and opinions derived from them in US Federal and State courts are based on criteria established by the US Supreme Court in the case of Daubert v. Merrell Dow and the 2000 Amendment of Rule 702 of the Federal Rules of Evidence. These criteria are being addressed by new efforts that include the development of certified reference materials (CRMs) to provide the basis for analytical method development, optimization, calibration, validation, quality control, testing, readiness, and declaration of measurement uncertainties. Quality data is crucial for all stages of the program, from R and D, and database development, to actual casework. Weakness at any point in the program can propagate to reduce the confidence of final conclusions. The new certified reference materials will provide the necessary means to demonstrate a high level of metrological rigor for nuclear forensics evidence and will form a foundation for legally defensible nuclear chemical analysis. The CRMs will allow scientists to devise validated analytical methods, which can be corroborated by independent analytical laboratories. CRMs are required for ISO accreditation of many different analytical techniques which may be employed in the analysis of interdicted nuclear materials. (author)

Metrological role of reactor neutron activation analysis in contemporary inorganic trace analysis

Energy Technology Data Exchange (ETDEWEB)

Tian Weizhi [China Institute of Atomic Energy, Beijing (China)

2003-03-01

In this paper, the inherent characteristics of relative instrumental neutron activation analysis (INAA) as a primary ratio method of measurement, the unique functions of parametric INAA as an ideal back-up method of the relative INAA, and the valuable role of INAA in characterization of sampling behavior of individual elements in certified reference materials (CRMs) will be discussed. In the second of this series, traceability and uncertainty of measurement results by k{sub 0}-INAA will be described. The role of k{sub 0}-INAA as a back-up to relative INAA will be discussed. In the final series, minimum sample size, usually 100 mg or larger, is often the only information given in certificates of the existing certified reference materials (CRMs) to describe sampling behavior. This value is not only too large to cope with the quality control (QC) requirements of microanalysis, but also too general to reflect the strong element-specific nature of sampling behavior of solid materials. The need for CRMs with sampling behavior characterized for individual elements is explained, and the unique role INAA can play in this aspect is described. (J.P.N.)

Metrological role of reactor neutron activation analysis in contemporary inorganic trace analysis

International Nuclear Information System (INIS)

Tian Weizhi

2003-01-01

In this paper, the inherent characteristics of relative instrumental neutron activation analysis (INAA) as a primary ratio method of measurement, the unique functions of parametric INAA as an ideal back-up method of the relative INAA, and the valuable role of INAA in characterization of sampling behavior of individual elements in certified reference materials (CRMs) will be discussed. In the second of this series, traceability and uncertainty of measurement results by k 0 -INAA will be described. The role of k 0 -INAA as a back-up to relative INAA will be discussed. In the final series, minimum sample size, usually 100 mg or larger, is often the only information given in certificates of the existing certified reference materials (CRMs) to describe sampling behavior. This value is not only too large to cope with the quality control (QC) requirements of microanalysis, but also too general to reflect the strong element-specific nature of sampling behavior of solid materials. The need for CRMs with sampling behavior characterized for individual elements is explained, and the unique role INAA can play in this aspect is described. (J.P.N.)

Preparation and certification of Sargasso seaweed reference material

Energy Technology Data Exchange (ETDEWEB)

Okamoto, Kensaku

1988-01-01

Sargasso seaweed reference material was prepared from Sargassum felvellum obtained from an unpolluted area in Japan. The sargasso samples were washed, freeze-dried, pulverized, sieved to pass a 80-mesh screen and finally homogenized. Collaborative studies on the elemental analysis of the sargasso reference material were performed using various analytical techniques. Certified values are provided for Ag, As, Ca, Cd, Co, Cu, Fe, K, Mg, Mn, Na, Pb, Rb, Sr, V and Zn, based on results of determinations by at least three independent analytical techniques. Reference values are reported for Al, Br, Cl, Cr, Cs, Hg, I, P, S, Sb, Sc, Se, Ti and U. The sargasso certified reference material contains high levels of alkali metals, alkaline earth metals, I, Br, As and U, while the concentration of trace elements may be considered to be at the lower end of the range of reported values for marine brown algae. The sargasso sample will be of practical use in marine and environmental sciences as a certified reference material having an elemental composition close to background levels.

IAEA AQCS catalogue for reference materials and intercomparison exercises 1998/1999

International Nuclear Information System (INIS)

1999-01-01

Fore more than thirty years the International Atomic Energy Agency (IAEA), through its Analytical Quality Control Services (AQCS) programme, has been assisting Member States' laboratories to maintain and improve the reliability of their analyses by organizing intercomparison exercises and by preparing and distributing biological, environmental and marine reference materials. The catalogue consists principally of two parts: The list of all available IAEA reference materials grouped into five categories: reference materials for radionuclides; reference materials for trace, minor and major elements, including oxides; reference materials for stable isotopes; reference materials for organic contaminants and methyl mercury containing materials. Lists of all available IAEA reference materials sorted by analytes. In addition information on recommended half-life data and suppliers of radioactive sources is provided. Planned intercomparisons are advertised and request forms for participation in intercomparisons are included. Forms for ordering reference materials, quality control spectra for gamma-spectrometry on diskettes and AQCS related publications are also provided

Analytical quality control service programme, intercomparison runs, certified reference materials, reference materials 1987-88

International Nuclear Information System (INIS)

1986-12-01

The purpose of the Analytical Quality Control Services (AQCS) programme provided by the IAEA, is to assist laboratories engaged in the analysis of nuclear, environmental, biological, and materials of marine origin for radionuclide, major, minor and trace elements, as well as stable isotopes using atomic and nuclear analytical techniques, to check the quality of their work. The tables give details of the intercomparison samples and reference materials distributed by the IAEA in the period 1987 to 1988. 2 tabs

Specimen preparation for nano-scale investigation of cementitious repair material.

Science.gov (United States)

Azarsa, Pejman; Gupta, Rishi

2018-04-01

Cementitious Repair Materials (CRMs) in the construction industry have been used for many decades now and has become a very important part of activities in cement world. The performance of some of these CRMs when applied to retrofitting concrete structural elements is also well documented. However, the characterization of some of the CRMs at the micro- and nano level is not fully documented. The first step to studying materials at the microscopic level is to be able to fabricate proper specimens for microscopy. In this study, a special and newly developed class of CRM was selected and fabricated by Focused Ion Beam (FIB) using well-known "Lift-out" technique. The prepared specimen was later examined using various analytical techniques such as energy dispersive x-ray analysis using one of the highest and most stable Scanning Transmission Electron Holography Microscopy (STEHM) around the world. This process enabled understanding of the composition, morphology, and spatial distribution of various phases of the CRM. It was observed that the microstructure consisted of a very fine, compact, and homogenous amorphous structure. X-ray analysis indicated that there was considerable deviation between the Si/Ca ratios for the hydrated product. Copyright © 2018 Elsevier Ltd. All rights reserved.

Guide to nondestructive assay standards: Preparation criteria, availability, and practical considerations

International Nuclear Information System (INIS)

Stewart, J.E.; Hsue, S.T.; Sampson, T.E.

1997-01-01

For certification and measurement control, nondestructive assay (NDA) instruments and methods used for verification measurement of special nuclear materials (SNMs) require calibrations based on certified reference materials (CRMs), or working reference materials (WRMs), traceable to the national system of measurements, and adequately characteristic of the unknowns. The Department of Energy Office of Safeguards and Security is sponsoring production of a comprehensive guide to preparation of NDA standards. The scope of the report includes preparation criteria, current availability of CRMs and WRMs, practical considerations for preparation and characterization, and an extensive bibliography. In preparing the report, based primarily on experience at Los Alamos, we have found that standards preparation is highly dependent on the particular NDA method being applied. We therefore include sections that contain information specific to commonly used neutron and gamma-ray NDA techniques. 16 refs., 4 figs., 2 tabs

Determination of carbon-14 in environmental level, solid reference materials

Energy Technology Data Exchange (ETDEWEB)

Blowers, Paul, E-mail: paul.blowers@cefas.co.uk [Cefas Lowestoft Laboratory, Pakefield Road, Lowestoft, Suffolk, NR33 0HT (United Kingdom); Caborn, Jane, E-mail: jane.a.caborn@nnl.co.uk [NNL, Springfields, Salwick, Preston, Lancashire, PR4 0XJ (United Kingdom); Dell, Tony [Veterinary Laboratories Agency, New Haw, Addlestone, Surrey, KT15 3NB (United Kingdom); Gingell, Terry [DSTL, Radiation Protection Services, Crescent Road, Alverstoke, Gosport, Hants, PO12 2DL (United Kingdom); Harms, Arvic [National Physical Laboratory, Hampton Road, Teddington, Middlesex, TW11 0LW (United Kingdom); Long, Stephanie [Radiological Protection Institute of Ireland, 3 Clonskeagh Square, Clonskeagh Road, Dublin 14, Ireland (United Kingdom); Sleep, Darren [Centre for Ecology and Hydrology, Lancaster Environment Centre, Library Avenue, Bailrigg, Lancaster, LA1 4AP (United Kingdom); Stewart, Charlie [UKAEA (Waste Management Group), Chemical Support Services, D1310/14, Dounreay, Thurso, Caithness, KW14 7TZ (United Kingdom); Walker, Jill [Radiocarbon Dating, The Old Stables, East Lockinge, Wantage, Oxon OX12 8QY (United Kingdom); Warwick, Phil E. [GAU-Radioanalytical, National Oceanography Centre Southampton, European Way, Southampton, SO14 3ZH (United Kingdom)

2011-10-15

An intercomparison exercise to determine the {sup 14}C activity concentrations in a range of solid, environmental level materials was conducted between laboratories in the UK. IAEA reference materials, C2, C6 and C7, and an in-house laboratory QA material were dispatched in 2006 to ten laboratories comprising of members of the Analyst Informal Working Group (AIWG) and one other invited party. The laboratories performed the determinations using a number of techniques, and using the results each one was evaluated in terms of levels of precision, sensitivity and limits of detection. The results of the study show that all techniques are capable of successfully analysing {sup 14}C in environmental level materials, however, a shortage of certified environmental reference materials exists. The suitability of the IAEA reference materials and other material for use as reference materials was also assessed.

Determination of carbon-14 in environmental level, solid reference materials

International Nuclear Information System (INIS)

Blowers, Paul; Caborn, Jane; Dell, Tony; Gingell, Terry; Harms, Arvic; Long, Stephanie; Sleep, Darren; Stewart, Charlie; Walker, Jill; Warwick, Phil E.

2011-01-01

An intercomparison exercise to determine the 14 C activity concentrations in a range of solid, environmental level materials was conducted between laboratories in the UK. IAEA reference materials, C2, C6 and C7, and an in-house laboratory QA material were dispatched in 2006 to ten laboratories comprising of members of the Analyst Informal Working Group (AIWG) and one other invited party. The laboratories performed the determinations using a number of techniques, and using the results each one was evaluated in terms of levels of precision, sensitivity and limits of detection. The results of the study show that all techniques are capable of successfully analysing 14 C in environmental level materials, however, a shortage of certified environmental reference materials exists. The suitability of the IAEA reference materials and other material for use as reference materials was also assessed.

Use of gamma spectrometry for analysis of three reference materials

International Nuclear Information System (INIS)

Kinova, L.

2004-01-01

All reference materials (Reference material A: weight = 49.23 g; Reference material B: weight = 36.08 g; Reference material C: weight = 26.18 g) were packed in 50 cm 3 polypropylene vials, sealed and measured consecutively three times at intervals of the average of 25 days. Low background gamma spectrometry system: HPGe detector with high energy resolution (FWHM for 1332 KeV of Co-60 is 1.9 KeV, Relative counting efficiency for the same energy is 21 %) was used. Results: All materials are of low activity and must be measured for a long time.The highest specific activity of a man-made radionuclides Cs-137 and Am-241 is in the material A. An instrumentally measurable activity of Pb-210 also can be observed in this material. Medium values are in the material B. The reference material C according to the specific activity seems to be a low natural radioactivity material with highest activity of natural nuclides Th-232 and Pa-234 (progeny of U-238). Conclusions: Gamma spectrometry is an useful tool for initial measurement of materials with low radioactivity. Such measurements give an orientation for the nuclides content and approximate activity in the material for the following radiochemical determinations

An outline of reference materials for analysis techniques in China

International Nuclear Information System (INIS)

Zhang Yuanxun; Qian Yine; Zhang Yongping; Tong Yongpeng

1994-01-01

This paper provides background information on the development in the field of reference materials in China. The major considerations in development of reference materials include homogeneity, stability, handling procedures and certification. Further it discusses the plans for development in the near future specific natural-matrix reference materials containing low levels of trace elements and having high degree of homogeneity

An outline of reference materials for analysis techniques in China

Energy Technology Data Exchange (ETDEWEB)

Yuanxun, Zhang; Yine, Qian; Yongping, Zhang; Yongpeng, Tong [Shanghai Institute of Nuclear Research, Academia Sinica (China)

1994-07-01

This paper provides background information on the development in the field of reference materials in China. The major considerations in development of reference materials include homogeneity, stability, handling procedures and certification. Further it discusses the plans for development in the near future specific natural-matrix reference materials containing low levels of trace elements and having high degree of homogeneity.

A new certified reference material for size analysis of nanoparticles

International Nuclear Information System (INIS)

Braun, Adelina; Kestens, Vikram; Franks, Katrin; Roebben, Gert; Lamberty, Andrée; Linsinger, Thomas P. J.

2012-01-01

A certified reference material, ERM-FD100, for quality assurance and validation of various nanoparticle sizing methods, was developed by the Institute for Reference Materials and Measurements. The material was prepared from an industrially sourced colloidal silica containing nanoparticles with a nominal equivalent spherical diameter of 20 nm. The homogeneity and stability of the candidate reference material was assessed by means of dynamic light scattering and centrifugal liquid sedimentation. Certification of the candidate reference material was based on a global interlaboratory comparison in which 34 laboratories participated with various analytical methods (DLS, CLS, EM, SAXS, ELS). After scrutinising the interlaboratory comparison data, 4 different certified particle size values, specific for the corresponding analytical method, could be assigned. The good comparability of results allowed the certification of the colloidal silica material for nanoparticle size analysis.

Reference materials for micro-analytical nuclear techniques

International Nuclear Information System (INIS)

Valkovic, V.; Zeisler, R.; Bernasconi, G.; Danesi, P.R.

1994-01-01

Direct application of many existing reference materials in micro-analytical procedures such as energy dispersive x-ray fluorescence (EDXRF), particle induced x-ray emission spectroscopy (PIXE) and ion probe techniques for the determination of trace elements is often impossible or difficult because: 1) other constituents present in large amounts interfere with the determination; 2) trace components are not sufficiently homogeneously distributed in the sample. Therefore specific natural-matrix reference materials containing very low levels of trace elements and having high degree of homogeneity are required for many micro-analytical procedures. In this report, selection of the types of environmental and biological materials which are suitable for micro-analytical techniques will be discussed. (author)

Biological and environmental reference materials in CENAM.

Science.gov (United States)

Arvizu-Torres, R; Perez-Castorena, A; Salas-Tellez, J A; Mitani-Nakanishi, Y

2001-06-01

Since 1994, when the NIST/NOAA Quality Assurance Program in Chemical Measurements was discussed in Queretaro, CENAM, the National Measurement Institute (NMI) of Mexico, has become involved in the development of reference materials. In the field of biological and environmental reference materials, in particular, the NORAMET collaboration program with NIST and NRC, and the North-American Environmental Cooperation signed among three free-trade treaty organizations, have greatly helped the development of the materials metrology program in the newly established CENAM. This paper describes some particularly significant efforts of CENAM in the development of biological and environmental reference materials, on the basis of inter-comparison studies organized with local and governmental environmental agencies of Mexico. In the field of water pollution CENAM has developed a practical proficiency testing (PT) scheme for field laboratories, as a part of registration by local government in the metropolitan area, according to the Mexican Ecological Regulation. The results from these eight PTs in the last 5 years have demonstrated that this scheme has helped ensure the reliability of analytical capability of more than 50 field laboratories in three states, Mexico, D.F., and the States of Mexico and Queretaro. Similar experience has been obtained for more than 70 service units of stack emission measurements in the three states in 1998 and 1999, as a result of the design of a PT scheme for reference gas mixtures. This PT scheme has been accomplished successfully by 30 analytical laboratories who provide monitoring services and perform research on toxic substances (Hg, methylmercury, PCB, etc.) in Mexico. To support these activities, reference samples have been produced through the NIST SRMs, and efforts have been made to increase CENAM's capability in the preparation of primary reference materials in spectrometric solutions and gas mixtures. Collaboration among NMIs has also

A blueprint for radioanalytical metrology CRMs, intercomparisons, and PE

International Nuclear Information System (INIS)

Inn, Kenneth G.W.; Kurosaki, Hiromu; Frechou, Carole; Gilligan, Chris; Jones, Robert; LaMont, Stephen; Leggitt, Jeff; Li Chunsheng; McCroan, Keith; Swatski, Ronald

2008-01-01

A workshop was held from 28 February to 2 March 2006 at the National Institute of Standards and Technology (NIST) to evaluate the needs for new directions for complex matrix reference materials certified for radionuclide content, interlaboratory comparisons and performance evaluation (PE) programs. The workshop identified new radioanalytical metrology thrust areas needed for environmental, radiobioassay, emergency consequence management, and nuclear forensics, attribution, nonproliferation, and safeguards

REFERENCE MATERIALS IN THE SPHERE OF USE OF ATOMIC ENERGY

Directory of Open Access Journals (Sweden)

V. A. Borisov

2015-01-01

Full Text Available The article describes the chronology of development of the system of reference materials in the nuclear industry of the Russian Federation. The basic documents used in the sphere of nuclear energy are described. The nomenclature of reference materials and feature of their application in the "Rosatom" is given. The prospects of development activities in the field of reference materials are formulated.

Development of natural matrix reference materials for monitoring environmental radioactivity

International Nuclear Information System (INIS)

Holmes, A.S.; Houlgate, P.R.; Pang, S.; Brookman, B.

1992-01-01

The Department of the Environment commissioned the Laboratory of the Government Chemist to carry out a contract on natural matrix reference materials. A survey of current availability of such materials in the western world, along with the UK's need, was conducted. Four suitable matrices were identified for production and validation. Due to a number of unforeseen problems with the collection, processing and validation of the materials, the production of the four identified reference materials was not completed in the allocated period of time. In the future production of natural matrix reference materials the time required, the cost and the problems encountered should not be underestimated. Certified natural matrix reference materials are a vital part of traceability in analytical science and without them there is no absolute method of checking the validity of measurement in the field of radiochemical analysis. (author)

Preparation and analysis of a marble reference material

International Nuclear Information System (INIS)

Carmo Freitas, M.; Moens, L.; Seabra e Barros, J.

1988-01-01

A 7 kg stone of a Carrara marble was reduced to grains smaller than 100 μm, mixed and homogenized in order to prepare a marble reference material. The homogeneity was tested for 16 elements by instrumental neutron activation analysis (INAA). Through a one-way analysis of variance based on several analyses of each of 15 bottles and within the same bottle, it was concluded that the inter-bottle heterogeneity is not greater than the intra-bottle heterogeneity. Results on the concentration of major and trace elements in the marble reference material, obtained by different laboratories and different techniques, are given. The limestone certified reference material KALKSTEIN KH was used to evaluate measurement accuracy, to intercalibrate laboratories, and to provide compatibility of measurement data. (author) 10 refs.; 12 tabs

Preparation of in-house graphite reference material for boron

International Nuclear Information System (INIS)

Kumar, Sanjukta A.; Venkatesh, K.; Swain, Kallola K.; Manisha, V.; Kamble, Granthali S.; Pandey, Shailaja P.; Remya Devi, P.S.; Ghosh, M.; Verma, R.

2016-05-01

Graphite is extensively used in nuclear technology. Boron concentration in graphite is one of the important parameters that decide its acceptability for nuclear applications. Reliable analytical methods are essential for the determination of boron in graphite at concentration about 5 mg kg -1 . Reference materials are used for validation of existing analytical methods and developing new methodologies. In view of the importance of determination of boron in graphite and unavailability of graphite reference material, an In-house graphite reference material was prepared in Analytical Chemistry Division. Graphite source material was procured, processed to obtain powder of ≤ 75 μm (200 mesh) and bottled. Procedures were developed for the determination of boron in graphite using inductively coupled plasma optical emission spectrometry (ICPOES) and inductively coupled plasma mass spectrometry (ICPMS) techniques. Homogeneity testing was carried out on the bottled units and boron content along with the combined and expanded uncertainties were established. The assigned boron concentration in the In-house graphite reference material is (7.3±0.46) mg kg -1 . (author)

Guide to nondestructive assay standards: Preparation criteria, availability, and practical considerations

International Nuclear Information System (INIS)

Hsue, S.T.; Stewart, J.E.; Sampson, T.E.; Butler, G.W.; Rudy, C.R.; Rinard, P.M.

1997-10-01

For certification and measurement control, nondestructive assay (NDA) instruments and methods used for verification measurements of special nuclear materials (SNMs) require calibrations based on certified reference materials (CRMs), or working reference materials (WRMs), traceable to the national system of measurements, and adequately characteristic of the unknowns. The Department of Energy Office of Safeguards and Security is sponsoring production of a comprehensive guide to preparation of NDA standards. The scope of the report includes preparation criteria, current availability of CRMs and WRMs, practical considerations for preparation and characterization, and an extensive bibliography. In preparing the report, based primarily on experience at Los Alamos, they have found that standards preparation is highly dependent on the particular NDA method being applied. They therefore include sections that contain information specific to commonly used neutron and gamma-ray NDA techniques. They also present approaches that are alternatives to, or minimize requirements for physical standards

Certification of a niobium metal reference material for neutron dosimetry (EC nuclear reference material 526)

International Nuclear Information System (INIS)

Ingelbrecht, C.; Pauwels, J.

1990-01-01

Niobium metal, of 99.999% nominal purity, in the form of 0.02 and 0.1 mm thick foil and of 0.5 mm diameter wire, has been certified for its tantalum mass fraction. The certified value of the tantalum mass fraction is 0.3 ± 0.09 mg. Kg -1 , and is based on 70 results obtained by six independent laboratories by neutron activation analysis or inductively coupled plasma mass spectrometry. The material is intended to be used as a reference material in neutron metrology

Internal quality control of neutron activation analysis laboratory

Energy Technology Data Exchange (ETDEWEB)

Kim, S. H.; Mun, J. H.; BaeK, S. Y.; Jung, Y. S.; Kim, Y. J. [KAERI, Taejon (Korea, Republic of)

2004-07-01

The importance for quality assurance and control in analytical laboratories has been emphasized, day by day. Internal quality control using certified reference materials(CRMs) can be one of effective methods for this purpose. In this study, 10 kinds of CRMs consisting of soil, sediment and biological matrix were analyzed. To evaluate the confidence of analytical results and the validation of testing method and procedure, the accuracy and the precision of the measured elements were treated statistically and the reproducibility was compared with those values produced before 2003.

Reference material IAEA 413: Major, minor and trace elements in algae

International Nuclear Information System (INIS)

2010-01-01

Reference materials are a basic requirement for any sort of quantitative chemical and radiochemical analysis. Laboratories need them for calibration and quality control throughout their analytical work. The IAEA started to produce reference materials in the early 1960s to meet the needs of the analytical laboratories in its Member States that required reference materials for quality control of their measurements. The initial efforts were focused on the preparation of environmental reference materials containing anthropogenic radionuclides for use by those laboratories employing nuclear analytical techniques. These reference materials were characterized for their radionuclide content through interlaboratory comparison involving a core group of some 10 to 20 specialist laboratories. The success of these early exercises led the IAEA to extend its activities to encompass both terrestrial and marine reference materials containing primordial radionuclides and trace elements. Today, the IAEA has more than 90 reference materials and maintains a customer base of about 5000 members from more than 85 Member States. Within the frame of IAEA activities in production and certification of RM, this report describes the certification of the IAEA 413: Major, minor and trace elements in algae. Details are given on methodologies and data evaluation

Instrumental neutron activation analysis of marine sediment in-house reference material

International Nuclear Information System (INIS)

Nazaratul Ashifa Abdullah Salim; Mohd Suhaimi Hamzah; Mohd Suhaimi Elias; Siong, W.B.; Shamsiah Abdul Rahman; Azian Hashim; Shakirah Abdul Shukor

2013-01-01

Reference materials play an important role in demonstrating the quality and reliability of analytical data. The advantage of using in-house reference materials is that they provide a relatively cheap option as compared to using commercially available certified reference material (CRM) and can closely resemble the laboratory routine test sample. A marine sediment sample was designed as an in-house reference material, in the framework of quality assurance and control (QA/QC) program of the Neutron Activation Analysis (NAA) Laboratory at Nuclear Malaysia. The NAA technique was solely used for the homogeneity test of the marine sediment sample. The CRM of IAEA- Soil 7 and IAEA- SL1 (Lake Sediment) were applied in the analysis as compatible matrix based reference materials for QA purposes. (Author)

Certification of a nickel metal reference material for neutron dosimetry (EC Nuclear Reference Material 521)

International Nuclear Information System (INIS)

Pauwels, J.

1988-01-01

Nickel metal, of 99.99 % nominal purity and natural isotopic composition, in the form of 0.1 mm thick foil and 0.5 mm diameter wire has been certified for its cobalt mass fraction. The certified value of cobalt (<0.1μg.g-1) is based on 38 results obtained by neutron activation analysis, emission spectrometry with inductively coupled plasma excitation and atomic absorption spectrometry, whereas the isotopic composition of the nickel was verified by thermal ionization mass spectrometry. The material is intended to be used as a reference material in neutron metrology

Certification of an aluminium metal reference material for neutron dosimetry (EC nuclear reference material 523)

International Nuclear Information System (INIS)

Pauwels, J.; Ingelbrecht, C.

1990-01-01

Aluminium metal of > 99.999% nominal purity in the form of 0.1 mm and 1 mm thick foil and of 1 mm diameter wire has been certified for its sodium mass fraction. The certified value of the sodium mass fraction ( -1 ) is based on 21 results from three laboratories using two different methods, which are neutron activation analysis and atomic absorption spectrometry. The overall purity was estimated using spark source mass spectrometry and neutron activation analysis. The material is intended to be used as a reference material in neutron metrology

Development of сertified reference materials set for opened porosity of solid substances and materials (imitators

Directory of Open Access Journals (Sweden)

E. P. Sobina

2016-01-01

Full Text Available The article deals with data of research for development of certified reference materials set for opened porosity of solid substances and materials (imitators (OPTB SO UNIIM Set Certified Reference Materials GSO 10583-2015. The certified values of opened porosity of metal cylinders were established by the method of hydrostatic weighing before and after boring of holes in. The certified reference materials are intended for calibration and verification of measuring instruments of opened porosity, based on the Boyle - Mariotte's law.

A 244Pu spike reference material CBNM IRM-042A

International Nuclear Information System (INIS)

Verbruggen, A.; Gallet, M.; Hendrickx, F.; Bievre, P. de

1991-01-01

An highly enriched 244 Pu isotopic reference material (CBNM IRM-042a) has been prepared and certified for 244 Pu isotope concentration. The certified value of (2.257 7 ± 0.004 4).10 18 atoms 242 Pu.kg -1 of solution has been established by isotope dilution mass spectrometry. The plutonium isotopic composition has been determined by thermal ionization mass spectrometry and calibration of these measurements by means of synthetic 242 Pu/ 239 Pu mixtures. The isotopic reference material is supplied in a sealed glass ampoule containing approximately 10 g of a 5M nitric acid solution at an approximate concentration of 1 μg Pu per g solution. This isotopic reference material is part of a systematic CBNM programme to supply spike isotopic reference materials of various isotopes at different concentrations

Reference materials and their role in quality assurance in environmental monitoring

International Nuclear Information System (INIS)

Cortes, Eduardo

2002-01-01

The importance of a good and routine quality control procedure for the analyses of environmental samples is presented. The use of Reference Materials as one simple procedure for validating analytical methodologies and determining the accuracy of analytical data is emphasized. The quality of the reference materials is also discussed as well as their selection and correct use. The convenience of preparing 'in-house' reference materials is discussed and attention is called to relevant aspects to be considered. An example of the preparation of a reference material is presented and some aspects of the procedure are discussed. (author)

Recent developments in the field of environmental reference materials at the JRC Ispra.

Science.gov (United States)

Muntau, H

2001-06-01

The production of reference materials for environmental analysis started in the Joint Research Centre at Ispra/Italy in 1972 with the objective of later certification by the BCR, but for obvious budget reasons only a fraction of the total production achieved at Ispra ever reached certification level, although all materials were produced according to the severe quality requirements requested for certified reference materials. Therefore, the materials not destinated to certification are in growing demand as inter-laboratory test materials and as laboratory reference materials, for internal quality control, e.g., by control charts. The history of reference material production within the Joint Research Centre is briefly reviewed and the latest additions described. New developments such as micro-scale reference materials intended for analytical methods requiring sample intakes at milligram or sub-milligram level and therefor not finding supply on the reference material market, and "wet" environmental reference materials, which meet more precisely the "real-world" environmental analysis conditions, are presented and the state-of-the-art discussed.

Challenges for development and provision of metrological quality control tools in nuclear safeguards, nuclear forensics and nuclear security

International Nuclear Information System (INIS)

Aregbe, Y.; Richter, S.; Jakopic, R.; Bauwens, J.; Truyens, J.; Sturm, M.; Bujak, R.; Eykens, R.; Kehoe, F.; Kuehn, H.; Hennessy, C.

2013-01-01

Joint advancements in quality control tools and measurement sciences of international reference and safeguards laboratories include: -) successful integration of the Modified Total Evaporation technique (MTE) as a new tool for routine thermal ionization mass spectrometry in nuclear safeguards and security, -) research and feasibility studies for the development of new materials standard, particularly for nuclear forensics (Certified Reference Materials - CRMs for age-dating), -) quality control tools to support the additional protocol and nuclear security (particle CRMs, NUSIMEP (inter-laboratory comparisons for U particle analysis), and -) scientific/technical advice, training and knowledge transfer. The European Safeguards Research and Development Association (ESARDA), the Institute of Nuclear Materials Management (INMM) and the CETAMA Commission from the French Commission of Atomic Energy and Alternative Energies (CEA/CETAMA) and the International Atomic Energy Agency (IAEA) Technical Meetings are the platforms to exchange views on the needs and challenges for new Quality Control tools for nuclear safeguards and security. The paper is followed by the slides of the presentation

Determination of ancient ceramics reference material by neutron activation analysis

International Nuclear Information System (INIS)

Li Huhou; Sun Jingxin; Wang Yuqi; Lu Liangcai

1986-01-01

Contents of trace elements in the reference material of ancient ceramics (KPS-1) were determined by means of activation analysis, using thermal neutron irradiation produced in nuclear reactor. KPS-1 favoured the analysis of ancient ceramics because it had not only many kinds of element but also appropriate contents of composition. The values presented here are reliable within the experimental precision, and have shown that the reference material had a good homogeneity. So KPS-1 can be used as a suitable reference material for the ancient ceramics analysis

Phosphated minerals to be used as radioactive reference materials

International Nuclear Information System (INIS)

Braganca, M.J.C.S.; Tauhata, L.; Clain, A.F.; Moreira, I.

2003-01-01

The production and the supplying of certified reference materials, or deliberated contaminated materials containing natural radionuclides for laboratories which analyses environmental samples are fundamentals for the correct measurements of their radioactive levels. This analysis quality represents a important step for the safeguards of the population health, and quality control of the imported and exported products, such as minerals, agricultural and raw materials. The phosphate rocks, containing significant concentrations of thorium, and used as raw material and fertilizers justified a study for better characterization and distinction to be used cas certified reference radioactive materials. Therefore, samples from the two carboanalytical-alkaline chimneys (Araxa and Catalao), and one from metasedimentar origin (Patos de Minas), distant 100 km from each other, were collected and chemical and cholecystographic characterized by optical emission, X-ray diffraction and fluorescence. The element concentrations were determined by neutron activation analysis, ICP-MS and ICP-AES. The results, after multivariate statistical analysis and study of correlations among elements, have shown geochemical similarities of the phosphates from Araxa and Catalao, and differences from Patos de Minas, despite of the geographic proximity. The concentration of thorium between 200 and 500 (mg/g) allows to use such minerals as reference materials

Certification of an iron metal reference material for neutron dosimetry (EC nuclear reference material 524)

International Nuclear Information System (INIS)

Ingelbrecht, C.; Pauwels, J.; Lievens, F.

1993-01-01

Iron metal, of > 99.996% nominal purity, in the form of 0.1 mm thick foil and of 0.5 mm diameter wire has been certified for its manganese and cobalt mass fractions. The certified value of the cobalt mass fraction ( -1 ) is based on 39 accepted results from five laboratories using two different methods. The certified value of the manganese mass fraction ( -1 ) is based on 41 accepted results from five laboratories using three different methods. The overall purity was also verified. The material is intended to be used as a reference material in neutron dosimetry. (authors). 8 refs., 9 tabs., 2 figs

Preparation and provisional certification of NBL Spectrographic Impurity Standards, CRM 123 (1-7) and 124 (1-7)

International Nuclear Information System (INIS)

Santoliquido, P.M.

1983-09-01

This report describes the design, production, and provisional certification of two new certified reference materials (CRMs): CRM No. 123 (1-7), U 3 O 8 containing 18 trace elements, and CRM No. 124 (1-7), U 3 O 8 containing 24 trace elements. The elements to be included and concentrations to be used were decided on the basis of information gathered from users of a previous CRM of this type, CRM No. 98 (1-7). The new CRMs were prepared by the addition of trace elements to high purity U 3 O 8 . Provisional certification was accomplished by an interlaboratory program in which four different laboratories analyzed the materials by carrier distillation dc arc emission spectrography

Material synthesis and evaluation of metrological characteristics of potassium fluozirconate certified reference material

Directory of Open Access Journals (Sweden)

D. G. Lisienko

2016-01-01

Full Text Available The relevance of the study. For metrological support of control methods for composition ofpotassium fluozirconate, used in the production of metallic zirconium, applied in various technical fields, including nuclear power, electronics, chemical engineering. The purpose: development of synthesis technology, and determination of metrological characteristics of certified reference material for composition ofpotassium fluozirconate (set, intended for metrological support of measuring element mass fraction: hafnium (Hf, silicon (Si, iron (Fe, aluminium (Al, chromium (Cr, tin (Sn, titanium (Ti in potassium fluozirconate. Research methods: X-ray diffraction, differential scanning colorimetry, thermogravimetric analysis, atomic-emission spectral analysis with arc excitation, mass spectral analysis, X-ray fluorescence analysis. Results. As a result of research a set of certified reference materials for composition of potassium fluozirconate is developed and produced. The CRM type is approved by Federal Agency on Technical Regulating and Metrology and registered in State Register of Approved Reference Material Types under number GSO 10593-2015.

Preparation of reference material for the measurement of natural radioactivity

International Nuclear Information System (INIS)

Ben Tekaya, Malik

2010-01-01

The objective of this work is to prepare reference material for the calibration of gamma spectrometry, alpha and XRF .Many procedures of chemical preparation and radiological analysis of a reference material from Triple Superphosphate were tested. Several techniques and methods of measurement were used. In addition to a description and validation of these procedures, a study of repeatability was conducted which resulted in a positive characterization of this material.

Homogeneity test of the ceramic reference materials for non-destructive quantitative

International Nuclear Information System (INIS)

Li Li; Fong Songlin; Zhu Jihao; Feng Xiangqian; Xie Guoxi; Yan Lingtong

2010-01-01

In order to study elemental composition of ancient porcelain samples, we developed a set of ceramic reference materials for non-destructive quantitative analysis. In this paper,homogeneity of Al, Si, K, Ca, Ti, Mn and Fe contents in the ceramic reference materials is investigated by EDXRF. The F test and the relative standard deviation are used to treat the normalized net counts by SPSS. The results show that apart from the DY2 and JDZ4 reference materials, to which further investigation would be needed, homogeneity of the DH, DY3, JDZ3, JDZ6, GY1, RY1, LQ4, YJ1, YY2 and JY2 meets the requirements of ceramic reference materials for non-destructive quantitative analysis. (authors)

Preparation and preliminary of two new Polish CRMs for inorganic trace analysis

International Nuclear Information System (INIS)

Dybczynski, R.; Danko, B.; Kulisa, K.; Maleszewska, E.; Polkowska-Motrenko, H.; Samczynski, Z.; Szopa, Z.

2004-01-01

Preparation and characterization of two new reference materials of biological origin, namely: Tea Leaves (INCT-TL-1) and Mixed Polish Herbs (INCT-MPH-2) is described. The raw materials were ground in an agate ball mill, sieved through a nylon sieve, collecting fraction of particle size: diameter ≤67 μm, and carefully homogenized. Preliminary homogeneity testing by XRF method and final checking of homogeneity by NAA after distribution of the materials into containers revealed that they are sufficiently homogeneous at least for sample size ≥100 mg. Both materials were prepared in amounts exceeding 40 kg and certified on the basis of a worldwide interlaboratory comparison, in which 109 laboratories from 19 countries participated. The method of data evaluation leading to assignment of certified values was essentially the same as that used previously in this Laboratory, but supplemented by additional data from the analysis of a CRM which was sent to the participants and analyzed by them along with the candidate reference materials. In addition the results for a few elements by very accurate developed methods in this Laboratory were obtained and used to support the certification process. Analytical uncertainties and stability uncertainties were quantified to arrive at combined uncertainties of the certified values. So far 18 elements in INCT-TL-1 and 21 in INCT-MPH-2 could be certified. (author)

[The water content reference material of water saturated octanol].

Science.gov (United States)

Wang, Haifeng; Ma, Kang; Zhang, Wei; Li, Zhanyuan

2011-03-01

The national standards of biofuels specify the technique specification and analytical methods. A water content certified reference material based on the water saturated octanol was developed in order to satisfy the needs of the instrument calibration and the methods validation, assure the accuracy and consistency of results in water content measurements of biofuels. Three analytical methods based on different theories were employed to certify the water content of the reference material, including Karl Fischer coulometric titration, Karl Fischer volumetric titration and quantitative nuclear magnetic resonance. The consistency of coulometric and volumetric titration was achieved through the improvement of methods. The accuracy of the certified result was improved by the introduction of the new method of quantitative nuclear magnetic resonance. Finally, the certified value of reference material is 4.76% with an expanded uncertainty of 0.09%.

Preparation of reference material for organochlorine pesticides in a herbal matrix.

Science.gov (United States)

Wong, Yiu Chung; Wong, Siu Kay; Kam, Tat Ting

2008-12-01

The development of reference material for four organochlorine pesticides, namely hexachlorobenzene and three isomers of hexachlorocyclohexane (alpha-hexachlorocyclohexane, beta-hexachlorocyclohexane and gamma-hexachlorocyclohexane), in a ginseng root sample is presented. Raw materials (Panax ginseng) were purchased from a local market and confirmed to contain certain levels of incurred organochlorine pesticide residues by a validated gas chromatography-mass selective detection method. A total of more than 300 bottles each containing 25 g of samples were prepared after the materials had been freeze-dried, milled and thoroughly mixed. The homogeneity and stability of samples from randomly selected bottles were verified and the reference values were characterized using a highly precise isotope dilution gas chromatography-mass spectrometry (ID-GCMS) method that was recently developed by our laboratory. The purity of standard organochlorine chemicals was determined against certified reference materials to establish the accuracy of the ID-GCMS analysis. The concentrations (+/- expanded uncertainty) of hexachlorobenzene, alpha-hexachlorocyclohexane, beta-hexachlorocyclohexane and gamma-hexachlorocyclohexane in the reference material were 0.198 +/- 0.015, 0.450 +/- 0.022, 0.213 +/- 0.011 and 0.370 +/- 0.032 mg kg(-1), respectively. A portion (70 bottles) of the samples was also used in a proficiency testing (PT) scheme for assessing the testing capabilities of field laboratories. The consensus mean values of the PT obtained from the 70 participants were on the same order but deviated by -2.7 to -14.1% from those of the assigned reference values. Because of the wide spread of participants' data (relative standard deviation ranging from 44 to 56%), the PT results were not included in the calculation of the assigned values of the reference materials. The materials served as suitable reference materials to ascertain the quality control and validation processes for the

Immune reactivity of candidate reference materials

NARCIS (Netherlands)

Fernandez-Rivas, Montserrat; Aalbers, Marja; Fötisch, Kay; de Heer, Pleuni; Notten, Silla; Vieths, Stefan; van Ree, Ronald

2006-01-01

Immune reactivity is a key issue in the evaluation of the quality of recombinant allergens as potential reference materials. Within the frame of the CREATE project, the immune reactivity of the natural and recombinant versions of the major allergens of birch pollen (Bet v 1), grass pollen (Phl p 1

Evaluation of a reference material for glycated haemoglobin

NARCIS (Netherlands)

Weykamp, CW; Penders, TJ; Muskiet, FAJ; vanderSlik, W

The use of lyophilized blood as a reference material for glycated haemoglobin was investigated with respect to IFCC criteria for calibrators and control materials. Ninety-two laboratories, using 11 methods, detected no changes in glycated haemoglobin content when the lyophilizate was stored for one

An in-house usage assessment of print reference materials in a ...

African Journals Online (AJOL)

The study investigated the utilization of print reference materials in a Nigerian hybrid medical school library, factors influencing utilization or under utilization, and if utilization commensurate with the library's prospect on the use of these materials. During the period of study, it was assumed that all reference materials pulled ...

Standard Reference Development of nuclear material for Tensile and Hardness Test Properties

International Nuclear Information System (INIS)

Choo, Y. S.; Kim, D. S.; Yoo, B. O.; Ahn, S. B.; Baik, S. J.; Chun, Y. B.; Kim, K. H.; Hong, K. P.; Ryu, W. S.

2007-12-01

Standard reference is a official approved data such a coefficient of physics, approved material properties, and etc., which should be analyzed and evaluated by scientific method to acquire official approval for accuracy and credibility of measured data and information. So it could be used broadly and continuously by various fields of nation and society. It is classified to effective standard reference, verified standard reference, and certified standard reference. There are sixteen fields in designated standard references such a physical chemistry field, material field, metal field, and the others. The standard reference of neutron irradiated nuclear structural material is classified to metal field. This report summarized the whole processes about data collection, data production, data evaluation and the suggestion of details evaluation technical standard for tensile and hardness properties, which were achieved by carry out the project 'nuclear material standard reference development' as a result

Standard Reference Development of nuclear material for Tensile and Hardness Test Properties

Energy Technology Data Exchange (ETDEWEB)

Choo, Y. S.; Kim, D. S.; Yoo, B. O.; Ahn, S. B.; Baik, S. J.; Chun, Y. B.; Kim, K. H.; Hong, K. P.; Ryu, W. S

2007-12-15

Standard reference is a official approved data such a coefficient of physics, approved material properties, and etc., which should be analyzed and evaluated by scientific method to acquire official approval for accuracy and credibility of measured data and information. So it could be used broadly and continuously by various fields of nation and society. It is classified to effective standard reference, verified standard reference, and certified standard reference. There are sixteen fields in designated standard references such a physical chemistry field, material field, metal field, and the others. The standard reference of neutron irradiated nuclear structural material is classified to metal field. This report summarized the whole processes about data collection, data production, data evaluation and the suggestion of details evaluation technical standard for tensile and hardness properties, which were achieved by carry out the project 'nuclear material standard reference development' as a result.

Certification of biological candidates reference materials by neutron activation analysis

Science.gov (United States)

Kabanov, Denis V.; Nesterova, Yulia V.; Merkulov, Viktor G.

2018-03-01

The paper gives the results of interlaboratory certification of new biological candidate reference materials by neutron activation analysis recommended by the Institute of Nuclear Chemistry and Technology (Warsaw, Poland). The correctness and accuracy of the applied method was statistically estimated for the determination of trace elements in candidate reference materials. The procedure of irradiation in the reactor thermal fuel assembly without formation of fast neutrons was carried out. It excluded formation of interfering isotopes leading to false results. The concentration of more than 20 elements (e.g., Ba, Br, Ca, Co, Ce, Cr, Cs, Eu, Fe, Hf, La, Lu, Rb, Sb, Sc, Ta, Th, Tb, Yb, U, Zn) in candidate references of tobacco leaves and bottom sediment compared to certified reference materials were determined. It was shown that the average error of the applied method did not exceed 10%.

Certification of a new biological reference material - Virginia Tobacco Leaves (CTA-VTL-2) and homogeneity study by NAA on this and other candidate reference materials

International Nuclear Information System (INIS)

Dybczynski, Rajmund; Polkowska-Motrenko, Halina; Samczynski, Zbigniew; Szopa, Zygmunt; Kulisa, Krzysztof; Wasek, Marek

2002-01-01

This report describes the laboratory's participation in the interlaboratory comparison run where the laboratory applied neutron activation analysis aimed at certification of the candidate reference material. Data evaluation and statistical treatment steps are discussed. The report also describes homogeneity study on the reference material and provides details of the analytical procedures

A new basaltic glass microanalytical reference material for multiple techniques

Science.gov (United States)

Wilson, Steve; Koenig, Alan; Lowers, Heather

2012-01-01

The U.S. Geological Survey (USGS) has been producing reference materials since the 1950s. Over 50 materials have been developed to cover bulk rock, sediment, and soils for the geological community. These materials are used globally in geochemistry, environmental, and analytical laboratories that perform bulk chemistry and/or microanalysis for instrument calibration and quality assurance testing. To answer the growing demand for higher spatial resolution and sensitivity, there is a need to create a new generation of microanalytical reference materials suitable for a variety of techniques, such as scanning electron microscopy/X-ray spectrometry (SEM/EDS), electron probe microanalysis (EPMA), laser ablation inductively coupled mass spectrometry (LA-ICP-MS), and secondary ion mass spectrometry (SIMS). As such, the microanalytical reference material (MRM) needs to be stable under the beam, be homogeneous at scales of better than 10–25 micrometers for the major to ultra-trace element level, and contain all of the analytes (elements or isotopes) of interest. Previous development of basaltic glasses intended for LA-ICP-MS has resulted in a synthetic basaltic matrix series of glasses (USGS GS-series) and a natural basalt series of glasses (BCR-1G, BHVO-2G, and NKT-1G). These materials have been useful for the LA-ICP-MS community but were not originally intended for use by the electron or ion beam community. A material developed from start to finish with intended use in multiple microanalytical instruments would be useful for inter-laboratory and inter-instrument platform comparisons. This article summarizes the experiments undertaken to produce a basalt glass reference material suitable for distribution as a multiple-technique round robin material. The goal of the analytical work presented here is to demonstrate that the elemental homogeneity of the new glass is acceptable for its use as a reference material. Because the round robin exercise is still underway, only

Element content and particle size characterization of a mussel candidate reference material

International Nuclear Information System (INIS)

Moreira, Edson G.; Vasconcellos, Marina B.A.; Santos, Rafaela G. dos; Martinelli, Jose R.

2011-01-01

The use of certified reference materials is an important tool in the quality assurance of analytical measurements. To assure reliability on recently prepared powder reference materials, not only the characterization of the property values of interest and their corresponding uncertainties, but also physical properties such as the particle size distribution must be well evaluated. Narrow particle size distributions are preferable than larger ones; as different size particles may have different analyte content. Due to this fact, the segregation of the coarse and the fine particles in a bottle may lead to inhomogeneity of the reference material, which should be avoided. In this study the element content as well as the particle size distribution of a mussel candidate reference material produced at IPEN-CNEN/SP was investigated. Instrumental Neutron Activation Analysis was applied to the determination of 15 elements in seven fractions of the material with different particle size distributions. Subsamples of the materials were irradiated simultaneously with elemental standards at the IEA-R1 research nuclear reactor and the induced gamma ray energies were measured in a hyperpure germanium detector. Three vials of the candidate reference material and three coarser fractions, collected during the preparation, were analyzed by Laser Diffraction Particle Analysis to determine the particle size distribution. Differences on element content were detected for fractions with different particle size distribution, indicating the importance of particle size control for biological reference materials. From the particle size analysis, Gaussian particle size distribution was observed for the candidate reference material with mean particle size μ = 94.6 ± 0.8 μm. (author)

Preparation and certification of rice flour reference materials for trace elements analysis

International Nuclear Information System (INIS)

Cho, Kyung Haeng; Park, Chang Joon; Woo, Jin Choon; Suh, Jung Ki; Han, Myung Sub; Lee, Jong Hae

1998-01-01

Rice flour reference materials were prepared from the unpolished rice grown in korea and certified for elemental composition. The reference materials consist of two samples containing normal and high level. The reference material at elevated level was prepared by spiking to the normal rice flour six toxic elements of As, Cd, Cu, Cr, Hg, Pb with 1.0μg/g on a dry weight basis. Homogeneity of the prepared materials was evaluated through the determination of Ca, Cu, Fe, Mn, Zn by instrumental neutron activation analysis (INAA) and atomic absorption spectrometry (AAS). Small variance of elemental composition among inter-bottled samples assured homogeneity of the prepared materials. The materials were decomposed by high pres-sure digestion and microwave digestion method. INAA, AAS, inductively coupled plasma-atomic absorption spectrometry (ICP-AES), ICP-mass spectrometry (MS) and vapour generation techniques were employed to analyze the reference materials. From this independent analytical results, the certified or reference values are determined for As, Ca, Cd, Cr, Cu, Fe, Hg, K, Mg, Mn, Mo, Na, P, Pb, Se, Zn

Micro-homogeneity evaluation of a bovine kidney candidate reference material

Energy Technology Data Exchange (ETDEWEB)

Castro, Liliana; Moreira, Edson G.; Vasconcellos, Marina B.A., E-mail: lcastroesnal@usp.br [Instituto de Pesquisas Energéticas e Nucleares (IPEN/CNEN-SP), São Paulo, SP (Brazil)

2017-07-01

The minimum sample intake for which a reference material remains homogeneous is one of the parameters that must be estimated in the homogeneity assessment study of reference materials. In this work, Instrumental Neutron Activation Analysis was used to evaluate this quantity in a bovine kidney candidate reference material. The mass fractions of 9 inorganic constituents were determined in subsamples between 1 and 2 mg in order to estimate the relative homogeneity factor (HE) and the minimum sample mass to achieve 5% and 10% precision on a 95% confidence level. Results obtained for H{sub E} in all the analyzed elements were satisfactory. The estimated minimum sample intake was between 2 mg and 40 mg, depending on the element. (author)

Characterization of nanoparticles as candidate reference materials

International Nuclear Information System (INIS)

Martins Ferreira, E.H.; Robertis, E. de; Landi, S.M.; Gouvea, C.P.; Archanjo, B.S.; Almeida, C.A.; Araujo, J.R. de; Kuznetsov, O.; Achete, C.A.

2013-01-01

We report the characterization of three different nanoparticles (silica, silver and multi-walled carbon nanotubes) as candidate reference material. We focus our analysis on the size distribution of those particles as measured by different microscopy techniques. (author)

Production and certification of reference materials

International Nuclear Information System (INIS)

Sarkis, Jorge Eduardo de S.; Kakazu, Mauricio H.; Hespanhol, Emilio Carlos B.; Martins, Elaine Arantes J.

1996-01-01

The reference materials used in analytical chemistry permit us to evaluate correctly the analytical producers as well as experimental set up. U 3 O 8 was produced at IPEN to be used as a secondary standard. We present the first results on U 3 O 8 and discuss the method, preparation, and characterization of that oxide. (author)

Certification of butyltins and phenyltins in marine sediment certified reference material by species-specific isotope-dilution mass spectrometric analysis using synthesized {sup 118}Sn-enriched organotin compounds

Energy Technology Data Exchange (ETDEWEB)

Inagaki, Kazumi; Takatsu, Akiko; Watanabe, Takuro; Aoyagi, Yoshie; Yarita, Takashi; Okamoto, Kensaku; Chiba, Koichi [National Institute of Advanced Industrial Science and Technology (AIST), Environmental Standard Section, National Metrology Institute of Japan (NMIJ), Tsukuba, Ibaraki (Japan)

2007-04-15

A new marine sediment certified reference material, NMIJ CRM 7306-a, for butyltin and phenyltin analysis has been prepared and certified by the National Metrological Institute of Japan at the National Institute of Advanced Industrial Science and Technology (NMIJ/AIST). Candidate sediment material was collected at a bay near industrial activity in Japan. After air-drying, sieving, and mixing the material was sterilized with {gamma}-ray irradiation. The material was re-mixed and packaged into 250 glass bottles (15 g each) and these were stored in a freezer at -30 C. Certification was performed by use of three different types of species-specific isotope-dilution mass spectrometry (SSID-MS) - SSID-GC-ICP-MS, SSID-GC-MS, and SSID-LC-ICP-MS, with {sup 118}Sn-enriched organotin compounds synthesized from {sup 118}Sn-enriched metal used as a spike. The {sup 118}Sn-enriched mono-butyltin (MBT), dibutyltin (DBT), and tributyltin (TBT) were synthesized as a mixture whereas the {sup 118}Sn-enriched di-phenyltin (DPhT) and triphenyltin (TPhT) were synthesized individually. Four different extraction methods, mechanical shaking, ultrasonic, microwave-assisted, and pressurized liquid extraction, were adopted to avoid possible analytical bias caused by non-quantitative extraction and degradation or inter-conversion of analytes in sample preparations. Tropolone was used as chelating agent in all the extraction methods. Certified values are given for TBT 44{+-}3 {mu}g kg{sup -1} as Sn, DBT 51 {+-} 2 {mu}g kg{sup -1} as Sn, MBT 67 {+-} 3 {mu}g kg{sup -1} as Sn, TPhT 6.9 {+-} 1.2 {mu}g kg{sup -1} as Sn, and DPhT 3.4 {+-} 1.2 {mu}g kg{sup -1} as Sn. These levels are lower than in other sediment CRMs currently available for analysis of organotin compounds. (orig.)

Biological and environmental reference materials for trace elements, nuclides and organic microcontaminants

International Nuclear Information System (INIS)

Cortes Toro, E.; Parr, R.M.; Clements, S.A.

1990-01-01

This report has been produced from a database on analytical reference materials of biological and environmental origin, which is maintained at the International Atomic Energy Agency. It is an updated version of an earlier report, published in 1985, which focussed mainly on reference materials for trace elements. In the present version of the report, reference materials for trace elements still constitute the major part of the data; however, information is also now included on a number of other selected analytes of relevance to IAEA programmes, i.e. radionuclides, stable isotopes and organic microcontaminants. The database presently contains 2,694 analyte values for 117 analytes in 116 biological and 77 environmental (non-biological) reference materials produced by 20 different suppliers. Additional information on the cost of the material, the unit size supplied, (weight or volume), and the minimum weight of material recommended for analysis is also provided (if available to the authors). It is expected that this report will help analysts to select the reference material that matches as closely as possible, with respect to matrix type and concentrations of the analytes of interest, the ''real'' samples that are to be analysed. Refs, 12 tabs

IAEA programme of natural matrix reference materials for the determination of radionuclides

International Nuclear Information System (INIS)

Strachnov, V.; Valkovic, V.; LaRosa, J.; Dekner, R.; Zeisler, R.

1993-01-01

The International Atomic Energy Agency has been providing analytical quality control services (AQCS) to its Member States since the 1960's. The AQCS programme distributes reference materials (RMs), organizes intercomparison runs, and provides training courses for quality assurance in chemical analysis and radioactivity measurements of food, biological, environmental and marine materials. This paper focusses on those aspects of the subject dealing with reference materials and intercomparison runs for the determination of radionuclides. Nineteen natural matrix reference materials are available for the determination of radionuclides. Twelve new intercomparison and reference materials are in preparation or under consideration. The radionuclides of interest include: K-40, Mn-54, Co-60, Sr-90, Tc-99, Ru-106, Ba-133, Cs-134, Cs-137, Pb-210, Ra-226, Th-228, Th-232, Pu-238, Pu-239 + 240. (orig.)

Preparation and certification of reference materials for the nuclear industry

International Nuclear Information System (INIS)

Wagner, J.F.

1994-01-01

CETAMA (Commission for the Establishment of Analytical Methods) of the Cea group is producing and certifying uranium and plutonium reference materials to meet the requirements of analytical laboratories in the nuclear industry. Reference materials are required at all stages in the fuel cycle: from extraction of uranium, purification, conversion, uranium enrichment, fuel fabrication until reprocessing of spent fuel, management and storage of waste. 3 tabs

Development studies of captopril certified reference material

Directory of Open Access Journals (Sweden)

Raquel Nogueira

2011-06-01

Full Text Available This paper describes the studies performed with the candidate Certified Reference Material (CRM of captopril, the first CRM of an active pharmaceutical ingredient (API in Brazil, including determination of impurities (organic, inorganic and volatiles, homogeneity testing, short- and long-term stability studies, calculation of captopril content using the mass balance approach, and estimation of the associated measurement uncertainty.Este artigo descreve os estudos realizados com o candidato a Material de Referência Certificado (MRC de captopril, primeiro MRC de fármacos no Brasil, incluindo a determinação de impurezas (orgânicas, inorgânicas e voláteis, testes de homogeneidade, testes de estabilidade de curta e longa duração, cálculo do teor de captopril por balanço de massa e estimativa da incerteza de medição associada ao valor certificado.

Preparation of an estuarine sediment quality control material for the determination of trace metals

Directory of Open Access Journals (Sweden)

Hatje Vanessa

2006-01-01

Full Text Available Quality Control Materials (QCM have being used routinely in daily laboratory work as a tool to fill the gap between need and availability of Certified Reference Materials (CRM. The QCM are a low-cost alternative to CRMs, and they are in high demand, especially, for the implementation of quality control systems in laboratories of several areas. This paper describes the preparation of a QCM for the determination of trace metals in estuarine sediments and the results of an interlaboratory exercise. Homogeneity and stability studies were performed and analysis of variance was carried out with the results. No statistical significant differences were observed in the concentrations of Co, Cr, Cu, Mn, Pb and Zn between- or within bottle results. Neither the storage nor temperature affected the results. Therefore, the QCM produced is considered homogeneous and stable and can be used for statistical control charts, evaluation of reproducibility and interlaboratory exercises.

Standard and reference materials for environmental science. Part 1. Technical memo

Energy Technology Data Exchange (ETDEWEB)

Cantillo, A.Y.

1995-11-01

This is the fourth edition of the catalog of reference materials suited for use in environmental science, originally compiled in 1986 for NOAA, IOC, and UNEP. The catalog lists more than 1200 reference materials from 28 producers and contains information about their proper use, sources, availability, and analyte concentrations. Indices are included for elements, isotopes, and organic compounds, as are cross references to CAS registry numbers, alternate names, and chemical structures of selected organic compounds.

Standard and reference materials for environmental science. Part 2. Technical memo

Energy Technology Data Exchange (ETDEWEB)

Cantillo, A.Y.

1995-11-01

This is the fourth edition of the catalog of reference materials suited for use in environmental science, originally compiled in 1986 for NOAA, IOC, and UNEP. The catalog lists more than 1200 reference materials from 28 producers and contains information about their proper use, sources, availability, and analyte concentrations. Indices are included for elements, isotopes, and organic compounds, as are cross references to CAS registry numbers, alternate names, and chemical structures of selected organic compounds.

Using Item Data for Evaluating Criterion Reference Measures with an Empirical Investigation of Index Consistency.

Science.gov (United States)

Meredith, Keith E.; Sabers, Darrell L.

Data required for evaluating a Criterion Referenced Measurement (CRM) is described with a matrix. The information within the matrix consists of the "pass-fail" decisions of two CRMs. By differentially defining these two CRMs, different concepts of reliability and validity can be examined. Indices suggested for analyzing the matrix are listed with…

Preparation and development of new Pu spike isotopic reference materials at IRMM

Energy Technology Data Exchange (ETDEWEB)

Jakopic, Rozle; Bauwens, Jeroen; Richter, Stephan; Sturm, Monika; Verbruggen, Andre; Wellum, Roger; Eykens, Roger; Kehoe, Frances; Kuehn, Heinz; Aregbe, Yetunde [Institute for Reference Materials and Measurements (IRMM) Joint Research Centre, European Commission, Geel, (Belgium)

2011-12-15

Reliable isotope measurements of nuclear material and the availability of reference materials with small uncertainties in the certified values are of great importance for safeguarding of nuclear materials. They provide the basis for a credible measurement system in the verification of states declarations of their nuclear activities. Worldwide needs for continued and improved Isotopic Reference Materials (IRM) are the main reason for developments of new nuclear reference materials at IRMM. Measurement capabilities of laboratories have evolved considerably over the years, along with progress in modern analytical techniques. Some plutonium reference materials, however, have been on the market for decades and they need to be re-certified to smaller uncertainties. Moreover, new reference materials with appropriately small uncertainties in the certified values need to be made available enabling measurement laboratories to reduce their combined measurement uncertainties. Such high quality plutonium isotopic reference materials are essential for laboratories striving to meet the International Target Values for Measurement Uncertainties in Safeguarding Nuclear Materials (ITVs). The preparation and the certification of such materials are demanding and challenging tasks that require state-of-theart measurement procedures and equipment. The Institute for Reference Materials and Measurements (IRMM) has repeatedly demonstrated its capabilities in plutonium analysis and represents one of the few institutes that supplies plutonium IRMs worldwide. An inter-calibration campaign has been set up at IRMM inter-linking selected plutonium spike IRMs. In the scope of this compatibility study, new reference materials have been prepared for Isotope Dilution Mass Spectrometry (IDMS) in nuclear fuel cycle measurements. A new series of large-sized dried (LSD) spikes, IRMM- 1027n, has been prepared and certified for plutonium and uranium amount content and isotopic composition. These mixed

Standard reference materials analysis for MINT Radiocarbon Laboratory

International Nuclear Information System (INIS)

Noraishah Othman; Kamisah Alias; Nasasni Nasrul

2004-01-01

As a follow-up to the setting up of the MINT Radiocarbon Dating facility. an exercise on the IAEA standard reference materials was carried out. Radiocarbon laboratories frequently used these 8 natural samples to verify their systems. The materials were either pretreated or analysed directly to determine the activity of 14 C isotopes of the five samples expressed in % Modern (pMC) terms and to make recommendations on further use of these materials. We present the results of the five materials and discuss the analyses that were undertaken. (Author)

Recommended reference materials for realization of physicochemical properties pressure-volume-temperature relationships

CERN Document Server

Herington, E F G

1977-01-01

Recommended Reference Materials for Realization of Physicochemical Properties presents recommendations of reference materials for use in measurements involving physicochemical properties, namely, vapor pressure; liquid-vapor critical temperature and critical pressure; orthobaric volumes of liquid and vapor; pressure-volume-temperature properties of the unsaturated vapor or gas; and pressure-volume-temperature properties of the compressed liquid. This monograph focuses on reference materials for vapor pressures at temperatures up to 770 K, as well as critical temperatures and critical pressures

AQCS intercomparison runs, reference materials 1991

International Nuclear Information System (INIS)

1991-01-01

The purpose of the Analytical Quality Control Services programme provided by the IAEA is to assist laboratories engaged in the analysis of nuclear, environmental, biological, and materials of marine origin for radionuclide, major, minor and trace elements, as well as stable isotopes using atomic and nuclear analytical techniques, to check the quality of their work. The determination of accuracy requires special procedures such as analysis to be carried out by as many different and independent methods, analysts and techniques as possible, control analysis with reference materials and participation in interlaboratory comparison studies. This document gives details of the specimens and samples which the IAEA intends to distribute in 1991. Tabs

Developing Potential New Reference Materials for Light Isotopes in Foodstuffs

Science.gov (United States)

Frew, Russell; Van Hale, Robert; Clarke, Dianne; Abrahim, Aiman; Resch, Christian; Mayr, Leopold; Cannavan, Andrew; Gröning, Manfred

2013-04-01

Measurements of subtle variations in stable isotope ratios provide the means for verifying food integrity in numerous ways. Adulterants usually have different isotopic composition so their presence in a food is readily detectable. Stable isotope measurements can also be used to determine the region of production of the food. In most cases the ability of stable isotope measurements to verify, or otherwise reject, the authenticity of the food is greatly enhanced by comparison of a result to a reference database. The more high-quality data in the database, the more statistical power is afforded by the comparison. A serious weakness at present is the lack of reference materials in food matrices available to the community. Thus researchers have to rely on in-house standards for calibration and quality assurance. The result is that there are numerous datasets published that may be internally consistent but it is exceedingly difficult to combine these datasets into a cohesive database. This is particularly important for measurements of the hydrogen isotopes. Here we present a survey of the stable isotope (^2H, ^13C and ^15N) composition of 12 Reference Materials from the International Atomic Energy Agency catalogue. All but one of these materials are plant matter and have been developed as reference materials for other applications such as radionuclide or trace element measurements. Thus they have been verified as suitable materials in terms of stability and homogeneity for those tests. The purpose of this work is to ascertain if they are similarly suitable as stable isotope reference materials. The results from our survey show that there is a wide range in elemental and isotopic composition among these materials. For example, the ^15N values range from-13.5‰ to +18.6‰ and the nitrogen elemental composition range is from 0.7% to 9.7%. The ^13C values range from -20‰ to -40‰ and the carbon elemental composition ranges from 15% to 47%. We are now in the process of

Determination of polybrominated diphenyl ethers in environmental standard reference materials

Energy Technology Data Exchange (ETDEWEB)

Stapleton, Heather M.; Schantz, Michele M.; Wise, Stephen A. [National Institute of Standards and Technology, Analytical Chemistry Division, Gaithersburg, MD (United States); Keller, Jennifer M.; Kucklick, John R. [National Institute of Standards and Technology, Analytical Chemistry Division, Hollings Marine Laboratory, Charleston, SC (United States); Leigh, Stefan D. [National Institute of Standards and Technology, Statistical Engineering Division, Gaithersburg, MD (United States)

2007-04-15

Standard reference materials (SRMs) are valuable tools in developing and validating analytical methods to improve quality assurance standards. The National Institute of Standards and Technology (NIST) has a long history of providing environmental SRMs with certified concentrations of organic and inorganic contaminants. Here we report on new certified and reference concentrations for 27 polybrominated diphenyl ether (PBDE) congeners in seven different SRMs: cod-liver oil, whale blubber, fish tissue (two materials), mussel tissue and sediment (two materials). PBDEs were measured in these SRMs, with the lowest concentrations measured in mussel tissue (SRM 1974b) and the highest in sediment collected from the New York/New Jersey Waterway (SRM 1944). Comparing the relative PBDE congener concentrations within the samples, we found the biota SRMs contained primarily tetrabrominated and pentabrominated diphenyl ethers, whereas the sediment SRMs contained primarily decabromodiphenyl ether (BDE 209). The cod-liver oil (SRM 1588b) and whale blubber (SRM 1945) materials were also found to contain measurable concentrations of two methoxylated PBDEs (MeO-BDEs). Certified and reference concentrations are reported for 12 PBDE congeners measured in the biota SRMs and reference values are available for two MeO-BDEs. Results from a sediment interlaboratory comparison PBDE exercise are available for the two sediment SRMs (1941b and 1944). (orig.)

Atomic spectrometry and trends in clinical laboratory medicine

Science.gov (United States)

Parsons, Patrick J.; Barbosa, Fernando

2007-09-01

Increasing numbers of clinical laboratories are transitioning away from flame and electrothermal AAS methods to those based on ICP-MS. Still, for many laboratories, the choice of instrumentation is based upon (a) the element(s) to be determined, (b) the matrix/matrices to be analyzed, and (c) the expected concentration(s) of the analytes in the matrix. Most clinical laboratories specialize in measuring Se, Zn, Cu, and Al in serum, and/or Pb, Cd, Hg, As, and Cr in blood and/or urine, while other trace elements (e.g., Pt, Au etc.) are measured for therapeutic purposes. Quantitative measurement of elemental species is becoming more widely accepted for nutritional and/or toxicological screening purposes, and ICP-MS interfaced with separation techniques, such as liquid chromatography or capillary electrophoresis, offers the advantage of on-line species determination coupled with very low detection limits. Polyatomic interferences for some key elements such as Se, As, and Cr require instrumentation equipped with dynamic reaction cell or collision cell technologies, or might even necessitate the use of sector field ICP-MS, to assure accurate results. Nonetheless, whatever analytical method is selected for the task, careful consideration must be given both to specimen collection procedures and to the control of pre-analytical variables. Finally, all methods benefit from access to reliable certified reference materials (CRMs). While a variety of reference materials (RMs) are available for trace element measurements in clinical matrices, not all can be classified as CRMs. The major metrological organizations (e.g., NIST, IRMM, NIES) provide a limited number of clinical CRMs, however, secondary reference materials are readily available from commercial organizations and organizers of external quality assessment schemes.

Atomic spectrometry and trends in clinical laboratory medicine

International Nuclear Information System (INIS)

Parsons, Patrick J.; Barbosa, Fernando

2007-01-01

Increasing numbers of clinical laboratories are transitioning away from flame and electrothermal AAS methods to those based on ICP-MS. Still, for many laboratories, the choice of instrumentation is based upon (a) the element(s) to be determined, (b) the matrix/matrices to be analyzed, and (c) the expected concentration(s) of the analytes in the matrix. Most clinical laboratories specialize in measuring Se, Zn, Cu, and Al in serum, and/or Pb, Cd, Hg, As, and Cr in blood and/or urine, while other trace elements (e.g., Pt, Au etc.) are measured for therapeutic purposes. Quantitative measurement of elemental species is becoming more widely accepted for nutritional and/or toxicological screening purposes, and ICP-MS interfaced with separation techniques, such as liquid chromatography or capillary electrophoresis, offers the advantage of on-line species determination coupled with very low detection limits. Polyatomic interferences for some key elements such as Se, As, and Cr require instrumentation equipped with dynamic reaction cell or collision cell technologies, or might even necessitate the use of sector field ICP-MS, to assure accurate results. Nonetheless, whatever analytical method is selected for the task, careful consideration must be given both to specimen collection procedures and to the control of pre-analytical variables. Finally, all methods benefit from access to reliable certified reference materials (CRMs). While a variety of reference materials (RMs) are available for trace element measurements in clinical matrices, not all can be classified as CRMs. The major metrological organizations (e.g., NIST, IRMM, NIES) provide a limited number of clinical CRMs, however, secondary reference materials are readily available from commercial organizations and organizers of external quality assessment schemes

Certification of a uranium-238 dioxide reference material for neutron dosimetry (EC nuclear reference material 501)

International Nuclear Information System (INIS)

Pauwels, J.; Lievens, F.; Ingelbrecht, C.

1989-01-01

Uranium-238 oxide of 99.999% isotopic and 99.98% chemical purity was transformed into dioxide spheres of nominal 0.5 and 1.0 mm diameter by gel precipitation and subsequent calcination under carbon dioxide and under argon containing 5% hydrogen at 1 125 K. The spheres were analysed by thermal ionization mass spectrometry, including isotope dilution, by gravimetry and by potentiometric titration. On the basis of these analyses, the uranium mass fraction was certified at 879.4 ± 2.8 g.kg -1 , and the 235 U/U - and 238 U/U abundances at 10.4 ± 0.5 mg.kg -1 and 999.9896 ± 0.0005 g.kg -1 , respectively. The material is intended to be used as a reference material in neutron metrology

Round robin testing of thermal conductivity reference materials

International Nuclear Information System (INIS)

Hulstrom, L.C.; Tye, R.P.; Smith, S.E.

1985-07-01

The Basalt Waste Isolation Project (BWIP), operated by Rockwell Hanford Operations, has a need to determine the thermal properties of basalt in the region being considered for a nuclear waste repository in basalt. Experimental data on thermal conductivity and its variation with temperature are information required for the characterization of basalt. To establish thermal conductivity values for the reference materials, an interlaboratory measurements program was undertaken. The program was planned to meet the objectives of performing an experimental characterization of the new stock and providing a detailed analysis of the results such that reference values of thermal conductivity could be determined. This program of measurements of the thermal conductivity of Pyrex 7740 and Pyroceram 9606 has produced recommended values that are within +- 1% of those accepted previously. These measurements together with those of density indicate that the present lots of material are similar to those previously available. Pyrex 7740 and Pyroceram 9606 can continue to be used with confidence as thermal conductivity reference materials for studies on rocks and minerals and other materials of similar thermal conductivity. The uncertainty range for Pyrex 7740 and Pyroceram 9606 up to 300 0 C is +- 10.3% and +- 5.6%, respectively. This range is similar to that indicated for the previously recommended values proposed some 18 years ago. It would appear that the overall state of the art in thermal conductivity measurements for materials in this range has changed little in the intervening years. The above uncertainties, which would have been greater had not three data sets been eliminated, are greater than those which are normally claimed for each individual method. Analyses of these differences through refinements in techniques and additional measurements to higher temperatures are required. 13 refs., 7 figs., 4 tabs

Antimony speciation analysis in sediment reference materials using high-performance liquid chromatography coupled to hydride generation atomic fluorescence spectrometry

International Nuclear Information System (INIS)

Potin-Gautier, M.; Pannier, F.; Quiroz, W.; Pinochet, H.; Gregori, I. de

2005-01-01

This work presents the development of suitable methodologies for determination of the speciation of antimony in sediment reference samples. Liquid chromatography with a post-column photo-oxidation step and hydride generation atomic fluorescence spectrometry as detection system is applied to the separation and determination of Sb(III), Sb(V) and trimethylantimony species. Post-column decomposition and hydride generation steps were studied for sensitive detection with the AFS detector. This method was applied to investigate the conditions under which speciation analysis of antimony in sediment samples can be carried out. Stability studies of Sb species during the extraction processes of solid matrices, using different reagents solutions, were performed. Results demonstrate that for the extraction yield and the stability of Sb species in different marine sediment extracts, citric acid in ascorbic acid medium was the best extracting solution for antimony speciation analysis in this matrix (between 55% and 65% of total Sb was recovered from CRMs, Sb(III) being the predominant species). The developed method allows the separation of the three compounds within 6 min with detection limits of 30 ng g -1 for Sb(III) and TMSbCl2 and 40 ng g -1 for Sb(V) in sediment samples

Certification of a copper metal reference material for neutron dosimetry. (EC nuclear reference material 522)

International Nuclear Information System (INIS)

Ingelbrecht, C.; Pauwels, J.; Lievens, F.

1993-01-01

Copper metal of ≥ 99.995% nominal purity in the form of 0.1 and 1.0 mm thick foil and 0.5 and 1.0 mm diameter wire has been certified for its cobalt and silver mass fractions. The certified values are -1 and 0.95 ± 0.04 mg.kg -1 respectively, based on 66 results for cobalt and 88 results for silver obtained by nine laboratories using three methods. This reference material, EC-NRM 522, is intended for reactor neutron dosimetry. (authors). 14 refs., 1 annexe, 10 tabs., 2 figs

U. S. programs on reference and advanced cladding/duct materials

International Nuclear Information System (INIS)

Bennett, J.W.; Holmes, J.J.; Laidler, J.J.

1977-05-01

Two coordinated national programs are presently in place in the United States for development of reference and advanced cladding and duct alloys for near-term and long-term LMFBR applications. A number of government, industrial and university laboratories are active participants in these two ERDA-sponsored programs. The programs are administered by ERDA through a task group organization, with each task group representing a particular technical activity and the membership of the task group drawn from among the laboratories with active involvement in that activity. Technical coordination of the two programs is provided by the Hanford Engineering Development Laboratory. The National Reference Cladding and Duct Program is charged with the responsibility for development of the required technology to permit full utilization of the reference material, 20 percent cold-worked Type 316 stainless steel, in early LMFBR core applications. The current schedule calls for full evaluation of FFTF-related design base data prior to full-power operation of FFTF in early 1980, followed by a confirmation in early 1983 of reference material performance capabilities for initial-core CRBRP applications. Comprehensive evaluation of reference material performance to commercial plant goal fluence levels will be complete by 1985. The National Advanced Alloy Development Program was instituted in 1974 with the objective to develop, by 1986, advanced cladding and duct materials compatible with advanced fuel systems having peak burnup capabilities up to 150 MWD/kg and doubling times of 15 years or less. Screening of a large number of potential alloys was completed in mid-1975, and there are presently 16 candidate alloys under active investigation

Analytical determination of Chemical Oxygen Demand in samples considered to be difficult to analyse: solid substrates and liquid samples with high suspended solid concentrations

DEFF Research Database (Denmark)

Raposo, Francisco; Fernández-Cegrí, V.; De la Rubia, M.A.

of a general standard method and high quality certified reference materials (CRMs), currently the traceability of the COD determination in such samples is not easy to check. Proficiency testing (PT) is a powerful tool that can be used to test the performance that the participant’s laboratories can achieve. Two...

Particle size studies in the preparation of AQCS reference materials

International Nuclear Information System (INIS)

Fajgelj, A.; Zeisler, R.; Benesch, T.; Dekner, R.

1994-01-01

Particle size determination is one of the important steps in the characterization of physical properties of each particulate material. However, particle size distribution effects also a chemical composition of the material in terms of homogeneity and representativeness of the sample, as well as allows or not a possible sub-sampling of the material. All this is of great importance in the preparation of reference materials for which the chemical composition and physical properties have to be extremely well characterized. In the present paper we intend to present same efforts which have been done by Analytical Quality Control Services (AQCS) of the International Atomic Energy Agency (IAEA) in the field of particle size determination in the production of reference materials. The Malvern product MasterSizer X, based on laser light scattering is used for this purpose and the technique is also shortly discussed. (author)

Certified reference materials of trace elements in water

Indian Academy of Sciences (India)

Many decisions regarding the suitability of material/products are based on the ... In the present scenario of globalization of economy, use of certified reference ... our national accreditation body, National Accreditation Board for Testing and ...

The development and evaluation of reference materials for food microbiology

NARCIS (Netherlands)

Veld, in 't P.

1998-01-01

Since 1986 the National Institute of Public Health and the Environment (RIVM) has worked on the development and evaluation of microbiological reference materials (RMs) with support from the European Communities Bureau of Reference (BCR), now called Standards Measurement and Testing

Reference materials for nondestructive assay of special nuclear material. Volume 1. Uranium oxide plus graphite powder

International Nuclear Information System (INIS)

Sprinkle, J.K.; Likes, R.N.; Parker, J.L.; Smith, H.A.

1983-10-01

This manual describes the fabrication of reference materials for use in gamma-ray-based nondestructive assay of low-density uranium-bearing samples. The sample containers are 2-l bottles. The reference materials consist of small amounts of UO 2 spread throughout a graphite matrix. The 235 U content ranges from 0 to 100 g. The manual also describes the far-field assay procedure used with low-resolution detectors

Assessment of international reference materials for isotope-ratio analysis (IUPAC Technical Report)

Science.gov (United States)

Brand, Willi A.; Coplen, Tyler B.; Vogl, Jochen; Rosner, Martin; Prohaska, Thomas

2014-01-01

Since the early 1950s, the number of international measurement standards for anchoring stable isotope delta scales has mushroomed from 3 to more than 30, expanding to more than 25 chemical elements. With the development of new instrumentation, along with new and improved measurement procedures for studying naturally occurring isotopic abundance variations in natural and technical samples, the number of internationally distributed, secondary isotopic reference materials with a specified delta value has blossomed in the last six decades to more than 150 materials. More than half of these isotopic reference materials were produced for isotope-delta measurements of seven elements: H, Li, B, C, N, O, and S. The number of isotopic reference materials for other, heavier elements has grown considerably over the last decade. Nevertheless, even primary international measurement standards for isotope-delta measurements are still needed for some elements, including Mg, Fe, Te, Sb, Mo, and Ge. It is recommended that authors publish the delta values of internationally distributed, secondary isotopic reference materials that were used for anchoring their measurement results to the respective primary stable isotope scale.

Certification of biological reference materials by instrumental neutron activation analysis

International Nuclear Information System (INIS)

Lanjewar, Mamata R.; Lanjewar, R.B.

2014-01-01

A multielemental instrumental neutron activation analysis (INAA) method by short and long irradiation has been employed for the determination of 21 minor and trace elements in two standard Reference Materials P-RBF and P-WBF from Institute of Radioecology and Applied Nuclear Techniques ,Czechoslovakia. Also some biological standards such as Bowen's kale, cabbage leaves (Poland) including wheat and rice flour samples of local origin were analysed. It is suggested that INAA is an ideal method for the certification of Reference Materials of Biological Matrices. (author)

Sustainability evaluation of essential critical raw materials: cobalt, niobium, tungsten and rare earth elements

Science.gov (United States)

Tkaczyk, A. H.; Bartl, A.; Amato, A.; Lapkovskis, V.; Petranikova, M.

2018-05-01

The criticality of raw materials has become an important issue in recent years. As the supply of certain raw materials is essential for technologically-advanced economies, the European Commission and other international counterparts have started several initiatives to secure reliable and unhindered access to raw materials. Such efforts include the EU Raw Materials Initiative, European Innovation Partnership on Raw Materials, US Critical Materials Institute, and others. In this paper, the authors present a multi-faceted and multi-national review of the essentials for the critical raw materials (CRMs) Co, Nb, W, and rare earth elements (REEs). The selected CRMs are of specific interest as they are considered relevant for emerging technologies and will thus continue to be of increasing major economic importance. This paper presents a ‘sustainability evaluation’ for each element, including essential data about markets, applications and recycling, and possibilities for substitution have been summarized and analysed. All the presented elements are vital for the advanced materials and processes upon which modern societies rely. These elements exhibit superior importance in ‘green’ applications and products subject to severe conditions. The annual production quantities are quite low compared to common industrial metals. Of the considered CRMs, only Co and REE gross production exceed 100 000 t. At the same time, the prices are quite high, with W and Nb being in the range of 60 USD kg‑1 and some rare earth compounds costing almost 4000 USD kg‑1. Despite valiant effort, in practice some of the considered elements are de facto irreplaceable for many specialized applications, at today’s technological level. Often, substitution causes a significant loss of quality and performance. Furthermore, possible candidates for substitution may be critical themselves or available in considerably low quantities. It can be concluded that one preferred approach for the

Reference material for radionuclides in sediment IAEA-384 (Fangataufa Lagoon sediment)

DEFF Research Database (Denmark)

Povinec, P.P.; Pham, M.K.; Sanchez-Cabeza, J.A.

2007-01-01

A reference material designed for the determination of anthropogenic and natural radionuclides in sediment, IAEA-384 (Fangataufa Lagoon sediment), is described and the results of certification are presented. The material has been certified for 8 radionuclides (K-40, Co-60, Eu-155, Th-230, U-238, ...... management of radioanalytical laboratories engaged in the analysis of radionuclides in the environment, as well as for the development and validation of analytical methods and for training purposes. The material is available from IAEA in 100 g units.......A reference material designed for the determination of anthropogenic and natural radionuclides in sediment, IAEA-384 (Fangataufa Lagoon sediment), is described and the results of certification are presented. The material has been certified for 8 radionuclides (K-40, Co-60, Eu-155, Th-230, U-238, Pu......-238, Pu239+240 and Am-241). Information values are given for 12 radionuclides (Sr-90, Cs-137, Pb-210 (Po-210), Ra-226, Ra-228, Th-232, U-234, U-235, Pu-239, Pu-240 and Pu-241). Less reported radionuclides include Th-228, U-236, Np-239 and Pu-242. The reference material may be used for quality...

Normalization Methods and Selection Strategies for Reference Materials in Stable Isotope Analyes. Review

Energy Technology Data Exchange (ETDEWEB)

Skrzypek, G. [West Australian Biogeochemistry Centre, John de Laeter Centre of Mass Spectrometry, School of Plant Biology, University of Western Australia, Crawley (Australia); Sadler, R. [School of Agricultural and Resource Economics, University of Western Australia, Crawley (Australia); Paul, D. [Department of Civil Engineering (Geosciences), Indian Institute of Technology Kanpur, Kanpur (India); Forizs, I. [Institute for Geochemical Research, Hungarian Academy of Sciences, Budapest (Hungary)

2013-07-15

Stable isotope ratio mass spectrometers are highly precise, but not accurate instruments. Therefore, results have to be normalized to one of the isotope scales (e.g., VSMOW, VPDB) based on well calibrated reference materials. The selection of reference materials, numbers of replicates, {delta}-values of these reference materials and normalization technique have been identified as crucial in determining the uncertainty associated with the final results. The most common normalization techniques and reference materials have been tested using both Monte Carlo simulations and laboratory experiments to investigate aspects of error propagation during the normalization of isotope data. The range of observed differences justifies the need to employ the same sets of standards worldwide for each element and each stable isotope analytical technique. (author)

Analytical method comparisons for the accurate determination of PCBs in sediments

Energy Technology Data Exchange (ETDEWEB)

Numata, M.; Yarita, T.; Aoyagi, Y.; Yamazaki, M.; Takatsu, A. [National Metrology Institute of Japan, Tsukuba (Japan)

2004-09-15

National Metrology Institute of Japan in National Institute of Advanced Industrial Science and Technology (NMIJ/AIST) has been developing several matrix reference materials, for example, sediments, water and biological tissues, for the determinations of heavy metals and organometallic compounds. The matrix compositions of those certified reference materials (CRMs) are similar to compositions of actual samples, and those are useful for validating analytical procedures. ''Primary methods of measurements'' are essential to obtain accurate and SI-traceable certified values in the reference materials, because the methods have the highest quality of measurement. However, inappropriate analytical operations, such as incomplete extraction of analytes or crosscontamination during analytical procedures, will cause error of analytical results, even if one of the primary methods, isotope-dilution, is utilized. To avoid possible procedural bias for the certification of reference materials, we employ more than two analytical methods which have been optimized beforehand. Because the accurate determination of trace POPs in the environment is important to evaluate their risk, reliable CRMs are required by environmental chemists. Therefore, we have also been preparing matrix CRMs for the determination of POPs. To establish accurate analytical procedures for the certification of POPs, extraction is one of the critical steps as described above. In general, conventional extraction techniques for the determination of POPs, such as Soxhlet extraction (SOX) and saponification (SAP), have been characterized well, and introduced as official methods for environmental analysis. On the other hand, emerging techniques, such as microwave-assisted extraction (MAE), pressurized fluid extraction (PFE) and supercritical fluid extraction (SFE), give higher recovery yields of analytes with relatively short extraction time and small amount of solvent, by reasons of the high

Standard and reference materials for marine science. Third edition. Technical memo

International Nuclear Information System (INIS)

Cantillo, A.Y.

1992-08-01

The third edition of the catalog of reference materials suited for use in marine science, originally compiled in 1986 for NOAA, IOC, and UNEP. The catalog lists close to 2,000 reference materials from sixteen producers and contains information about their proper use, sources, availability, and analyte concentrations. Indices are included for elements, isotopes, and organic compounds, as are cross references to CAS registry numbers, alternate names, and chemical structures of selected organic compounds. The catalog is being published independently by both NOAA and IOC/UNEP and is available from NOAA/NOS/ORCA in electronic form

Three New Offset {delta}{sup 11}B Isotope Reference Materials for Environmental Boron Isotope Studies

Energy Technology Data Exchange (ETDEWEB)

Rosner, M. [BAM Federal Institute for Materials Research and Testing, Berlin (Germany); IsoAnalysis UG, Berlin (Germany); Vogl, J. [BAM Federal Institute for Materials Research and Testing, Berlin (Germany)

2013-07-15

The isotopic composition of boron is a well established tool in various areas of science and industry. Boron isotope compositions are typically reported as {delta}{sup 11}B values which indicate the isotopic difference of a sample relative to the isotope reference material NIST SRM 951. A significant drawback of all of the available boron isotope reference materials is that none of them covers a natural boron isotope composition apart from NIST SRM 951. To fill this gap of required {delta}{sup 11}B reference materials three new solution boric acid reference materials were produced, which cover 60 per mille of the natural boron isotope variation (-20 to 40 per mille {delta}{sup 11}B) of about 100 per mille . The new reference materials are certified for their {delta}{sup 11}B values and are commercially available through European Reference Materials (http://www.erm-crm.org). The newly produced and certified boron isotope reference materials will allow straightforward method validation and quality control of boron isotope data. (author)

Newly developed standard reference materials for organic contaminant analysis

Energy Technology Data Exchange (ETDEWEB)

Poster, D.; Kucklick, J.; Schantz, M.; Porter, B.; Wise, S. [National Inst. of Stand. and Technol., Gaithersburg, MD (USA). Center for Anal. Chem.

2004-09-15

The National Institute of Standards and Technology (NIST) has issued a number of Standard Reference Materials (SRM) for specified analytes. The SRMs are biota and biological related materials, sediments and particle related SRMs. The certified compounds for analysis are polychlorinated biphenyls (PCB), polycylic aromatic hydrocarbons (PAH) and their nitro-analogues, chlorinated pesticides, methylmercury, organic tin compounds, fatty acids, polybrominated biphenyl ethers (PBDE). The authors report on origin of materials and analytic methods. (uke)

Biological and environmental reference materials in neutron activation analysis work

International Nuclear Information System (INIS)

Guinn, V.P.; Gavrilas, M.

1990-01-01

The great usefulness of reference materials, especially ones of certified elemental composition, is discussed with particular attention devoted to their use in instrumental neutron activation analysis (INAA) work. Their use, including both certified and uncertified values, in calculations made by the INAA Advance Prediction Computer Program (APCP) is discussed. The main features of the APCP are described, and mention is made of the large number of reference materials run on the APCP (including the new personal computer version of the program), with NBS Oyster Tissue SRM-1566 used as the principal examle. (orig.)

On criteria for examining analysis quality with standard reference material

International Nuclear Information System (INIS)

Yang Huating

1997-01-01

The advantages and disadvantages and applicability of some criteria for examining analysis quality with standard reference material are discussed. The combination of the uncertainties of the instrument examined and the reference material should be determined on the basis of specific situations. Without the data of the instrument's uncertainty, it would be applicable to substitute the standard deviation multiplied by certain times for the uncertainty. The result of the examining should not result in more error reported in routine measurements than it really is. Over strict examining should also be avoided

Lawrence Livermore National Laboratory Working Reference Material Production Pla

Energy Technology Data Exchange (ETDEWEB)

Wong, Amy; Thronas, Denise; Marshall, Robert

1998-11-04

This Lawrence Livermore National Laboratory (LLNL) Working Reference Material Production Plan was written for LLNL by the Los Alamos National Laboratory to address key elements of producing seven Pu-diatomaceous earth NDA Working Reference Materials (WRMS). These WRMS contain low burnup Pu ranging in mass from 0.1 grams to 68 grams. The composite Pu mass of the seven WRMS was designed to approximate the maximum TRU allowable loading of 200 grams Pu. This document serves two purposes: first, it defines all the operations required to meet the LLNL Statement of Work quality objectives, and second, it provides a record of the production and certification of the WRMS. Guidance provided in ASTM Standard Guide C1128-89 was used to ensure that this Plan addressed all the required elements for producing and certifying Working Reference Materials. The Production Plan was written to provide a general description of the processes, steps, files, quality control, and certification measures that were taken to produce the WRMS. The Plan identifies the files where detailed procedures, data, quality control, and certification documentation and forms are retained. The Production Plan is organized into three parts: a) an initial section describing the preparation and characterization of the Pu02 and diatomaceous earth materials, b) middle sections describing the loading, encapsulation, and measurement on the encapsulated WRMS, and c) final sections describing the calculations of the Pu, Am, and alpha activity for the WRMS and the uncertainties associated with these quantities.

Initiative to manufacture and characterize Baculovirus Reference Material

NARCIS (Netherlands)

Kamen, A.; Aucoin, M.; Merten, O.W.; Alves, P.C.M.; Hashimoto, Y.; Airenne, K.; Hu, Y.C.; Mezzina, M.; Oers, van M.M.

2011-01-01

This letter to the editor brings to the attention of researchers an initiative to develop a baculovirus reference material repository. To be successful this initiative needs the support of a broad panel of researchers working with baculovirus vectors for recombinant protein production and gene

Assessment of a dynamic reference material for calibration of full-field measurement systems

Science.gov (United States)

Hack, Erwin; Feligiotti, Mara; Davighi, Andrea; Whelan, Maurice; Wang, Weizhuo V.; Patterson, Eann A.

2012-10-01

For holography and speckle interferometry the calibration of the sensitivity is a must, because illumination and observation directions vary across the field of view. A numerical estimate or a static calibration using rigid body motions is standard, and reference materials exist for static strain calibration. Recently, reference materials for the dynamic calibration of optical instruments of displacement and strain measurement were designed and prototypes were manufactured in the European FP7 project ADVISE. We review the properties of the reference material and the concept of traceability for the field of displacement values by using a calibrated single point transducer. The mode shape is assessed using out-of-plane DSPI, Finite Element Analysis as well as analytic solutions of the plate vibration. We present measurements using stroboscopic DSPI on the reference material under acoustic excitation and compare the measured mode shapes to the ones predicted by FE analysis. We apply different comparison methodologies based on point-by-point deviations and on decomposition of the mode shapes into a set of orthogonal basis functions. The latter method is well suited to assess stability and reproducibility of a mode shape. Finally, the deviations are used to estimate the reference material uncertainty which is an essential parameter for determining the calibration uncertainty. Uncertainty contributions of the DSPI set-up are taken into account. To conclude, the application area and limitations of the reference material are discussed.

Role of neutron activation analysis in metrology of modern inorganic trace analysis. Pt.3: NAA in characterization of sampling behavior for multielements

International Nuclear Information System (INIS)

Tian Weizhi; Ni Bangfa; Wang Pingsheng; Chen Xilin; Huang Donghui; Zhang Guiying; Zhang Lanzhi; Liu Cunxiong; Liu Likun

2005-01-01

The necessity of the development of new generation of certified reference materials (CEMs) and the role that NAA will play in the certification of those CRMs are discussed. In conclusion, the major role of NAA in the metrology of contemporary inorganic trace analysis is summarized: the international recognition of NAA as a primary ratio method will imply a major contribution to the improvement of CEMs: the concurrent use of k 0 -NAA will further strengthen the position of relative NAA as a primary ratio method; and NAA will play an irreplaceable role in the creation of new generation of CRMs, that will eventually lead the establishment of quality control system for microanalysis. (authors)

A Reference Guide for Cryogenic Properties of Materials

Energy Technology Data Exchange (ETDEWEB)

Weisend, John G

2003-09-16

A thorough knowledge of the behavior of materials at cryogenic temperatures is critical for the design of successful cryogenic systems. Over the past 50 years, a tremendous amount of material properties at cryogenic temperatures have been measured and published. This guide lists resources for finding these properties. It covers online databases, computer codes, conference proceedings, journals, handbooks, overviews and monographs. It includes references for finding reports issued by government laboratories and agencies. Most common solids and fluids used in cryogenics are covered.

Uranium tailings reference materials

International Nuclear Information System (INIS)

Smith, C.W.; Steger, H.F.; Bowman, W.S.

1984-01-01

Samples of uranium tailings from Bancroft and Elliot Lake, Ontario, and from Beaverlodge and Rabbit Lake, Saskatchewan, have been prepared as compositional reference materials at the request of the National Uranium Tailings Research Program. The four samples, UTS-1 to UTS-4, were ground to minus 104 μm, each mixed in one lot and bottled in 200-g units for UTS-1 to UTS-3 and in 100-g units for UTS-4. The materials were tested for homogeneity with respect to uranium by neutron activation analysis and to iron by an acid-decomposition atomic absorption procedure. In a free choice analytical program, 18 laboratories contributed results for one or more of total iron, titanium, aluminum, calcium, barium, uranium, thorium, total sulphur, and sulphate for all four samples, and for nickel and arsenic in UTS-4 only. Based on a statistical analysis of the data, recommended values were assigned to all elements/constituents, except for sulphate in UTS-3 and nickel in UTS-4. The radioactivity of thorium-230, radium-226, lead-210, and polonium-210 in UTS-1 to UTS-4 and of thorium-232, radium-228, and thorium-228 in UTS-1 and UTS-2 was determined in a radioanalytical program composed of eight laboratories. Recommended values for the radioactivities and associated parameters were calculated by a statistical treatment of the results

10 CFR 433.3 - Materials incorporated by reference.

Science.gov (United States)

2010-01-01

... 10 Energy 3 2010-01-01 2010-01-01 false Materials incorporated by reference. 433.3 Section 433.3 Energy DEPARTMENT OF ENERGY ENERGY CONSERVATION ENERGY EFFICIENCY STANDARDS FOR THE DESIGN AND...) 741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations...

Approved reference and testing materials for use in Nuclear Waste Management Research and Development Programs

International Nuclear Information System (INIS)

Mellinger, G.B.; Daniel, J.L.

1984-12-01

This document, addressed to members of the waste management research and development community summarizes reference and testing materials available from the Nuclear Waste Materials Characterization Center (MCC). These materials are furnished under the MCC's charter to distribute reference materials essential for quantitative evaluation of nuclear waste package materials under development in the US. Reference materials with known behavior in various standard waste management related tests are needed to ensure that individual testing programs are correctly performing those tests. Approved testing materials are provided to assist the projects in assembling materials data base of defensible accuracy and precision. This is the second issue of this publication. Eight new Approved Testing Materials are listed, and Spent Fuel is included as a separate section of Standard Materials because of its increasing importance as a potential repository storage form. A summary of current characterization information is provided for each material listed. Future issues will provide updates of the characterization status of the materials presented in this issue, and information about new standard materials as they are acquired. 7 references, 1 figure, 19 tables

Survey of reference materials for trace elements, nuclides and organic microcontaminants

International Nuclear Information System (INIS)

Parr, R.M.; Stone, S.F.; Bel-Amakeletch, T.; Zeisler, R.

1998-01-01

The International Atomic Energy Agency (IAEA), in co-operation with the United Nations Environment Programme (UNEP), has recently prepared a survey on internationally available analytical reference materials for trace elements, nuclides and organic contaminants in biological, environmental and related matrices. The purpose is to help analysts to select reference materials for quality assurance that match as closely as possible, with respect to matrix type and concentrations of the measurands of interest, the ''real'' samples that are to be measured. The present version of the survey, which is available in the form of two cost-free printed volumes [1], contains over 10,000 certified and information values in 650 reference materials from 27 different producers. The 455 measurands listed include trace elements, major and minor elements, organic contaminants, organometallic compounds, radionuclides and stable isotopes. Currently, the database from which the survey has been produced is being modified and extended so as to make the data available in electronic form via the Internet. (orig.)

Preparation of gaseous CRMs from the primary system for "2"2"2Rn activity measurement

International Nuclear Information System (INIS)

Kim, B.J.; Kim, B.C.; Lee, K.B.; Lee, J.M.; Park, T.S.

2016-01-01

For disseminating the gaseous radon standard traceable to the KRISS primary system based on the defined solid angle counting method, two kinds of radon CRM (a glass ampule type and a stainless steel cylinder type) were developed. The activity of the CRM was certified by subtracting a residual activity from the measured activity by the primary system. After certification, the ampule CRM was used to calibrate a radon-monitoring instrument and the cylinder CRM to calibrate an HPGe system. We also improved the measurement procedure of the radon primary system. In a typical radon energy spectrum, the radon peak overlaps with the polonium peak. For more reliable and accurate measurement of radon activity, a fitting method was adopted for the evaluation of radon area in the alpha energy spectrum. The result of radon activity evaluated by using the fitting method is in good agreement with that by the previous integration method. - Highlights: • Preparation of gaseous Rn-222 CRMs from primary measurement system. • Convolution of 3 left-handed exponentials with a Gaussian function to count radon. • Calibration of continuous radon monitor using glass ampoule CRM. • Calibration of HPGe system as secondary standard for stainless steel cylinder CRM.

The influence of pyrolysis and matrix modifiers on determination of Cr and Pb in sediment samples by GFAAS

Directory of Open Access Journals (Sweden)

Risfidian Mohadi

2016-04-01

Full Text Available Abstract: The Influence of pyrolysis and matrix modifiers on determination of Cr and Pb in sediment samples using graphite furnace atomic absorption spectrometry has been investigated. The sediment samples including three certified reference materials (CRMs are reported. Analyses were performed using microwave assisted dissolution. The matrix modifiers Mg(NO32, Pd+Mg(NO32 and NH4H2PO4were shown to be optimazed. The recovery for Cr and Pb in CRMs in the case of sample dissolution was found to be between 81 to 91% for Cr and 94 to 98% for Pb of the certified values, respectively. Keywords: Sediment, Pyrolysis, Matrix modifiers, Cr, Pb Abstrak (Indonesia: Pengaruh pirolisis dan matriks pengubah pada penentuan Cr dan Pb dalam sampel sedimen menggunakan tungku grafit spektroskopi serapan atom telah diteliti. Sampel sedimen termasuk tiga bahan referensi bersertifikat (CRMs dilaporkan dianalisis dengan menggunakan bantuan microwave ekstraktor. Matriks pengubah Mg(NO32, Pd+Mg(NO32 dan NH4H2PO4 telah digunakan dan menghasilkan nilai temu balik untuk Cr dan Pb dalam CRMs ditemukan antara 81-91% untuk Cr dan 94-98 % untuk Pb dari nilai sertifikat masing-masing. Katakunci: Sedimen, Pirolisis, Matrix modifiers, Cr, Pb

Soiled-based uranium disequilibrium and mixed uranium-thorium series radionuclide reference materials

International Nuclear Information System (INIS)

Donivan, S.; Chessmore, R.

1988-12-01

The US Department of Energy (DOE) Office of Remedial Action and Waste Technology has assigned the Technical Measurements Center (TMC), located at the DOE Grand Junction Colorado, Projects Office and operated by UNC Geotech (UNC), the task of supporting ongoing remedial action programs by providing both technical guidance and assistance in making the various measurements required in all phases of remedial action work. Pursuant to this task, the Technical Measurements Center prepared two sets of radionuclide reference materials for use by remedial action contractors and cognizant federal and state agencies. A total of six reference materials, two sets comprising three reference materials each, were prepared with varying concentrations of radionuclides using mill tailings materials, ores, and a river-bottom soil diluent. One set (disequilibrium set) contains varying amounts of uranium with nominal amounts of radium-226. The other set (mixed-nuclide set) contains varying amounts of uranium-238 and thorium-232 decay series nuclides. 14 refs., 10 tabs

Evaluation of Botanical Reference Materials for the Determination of Vanadium in Biological Samples

DEFF Research Database (Denmark)

Heydorn, Kaj; Damsgaard, Else

1982-01-01

Three botanical reference materials prepared by the National Bureau of Standards have been studied by neutron activation analysis to evaluate their suitability with respect to the determination of vanadium in biological samples. Various decomposition methods were applied in connection with chemic....... A reference value of 1.15 mg/kg of this material is recommended, based on results from 3 different methods. All three materials are preferable to SRM 1571 Orchard Leaves, while Bowen's Kale remains the material of choice because of its lower concentration....

Normalization Methods and Selection Strategies for Reference Materials in Stable Isotope Analyses - Review

International Nuclear Information System (INIS)

Skrzypek, G.; Sadler, R.; Paul, D.; Forizs, I.

2011-01-01

A stable isotope analyst has to make a number of important decisions regarding how to best determine the 'true' stable isotope composition of analysed samples in reference to an international scale. It has to be decided which reference materials should be used, the number of reference materials and how many repetitions of each standard is most appropriate for a desired level of precision, and what normalization procedure should be selected. In this paper we summarise what is known about propagation of uncertainties associated with normalization procedures and propagation of uncertainties associated with reference materials used as anchors for the determination of 'true' values for δ''1''3C and δ''1''8O. Normalization methods Several normalization methods transforming the 'raw' value obtained from mass spectrometers to one of the internationally recognized scales has been developed. However, as summarised by Paul et al. different normalization transforms alone may lead to inconsistencies between laboratories. The most common normalization procedures are: single-point anchoring (versus working gas and certified reference standard), modified single-point normalization, linear shift between the measured and the true isotopic composition of two certified reference standards, two-point and multipoint linear normalization methods. The accuracy of these various normalization methods has been compared by using analytical laboratory data by Paul et al., with the single-point and normalization versus tank calibrations resulting in the largest normalization errors, and that also exceed the analytical uncertainty recommended for δ 13 C. The normalization error depends greatly on the relative differences between the stable isotope composition of the reference material and the sample. On the other hand, the normalization methods using two or more certified reference standards produces a smaller normalization error, if the reference materials are bracketing the whole range of

APEX (Air Pollution Exercise) Volume 20: Reference Materials.

Science.gov (United States)

Environmental Protection Agency, Research Triangle Park, NC. Office of Manpower Development.

The Reference Materials Manual is part of a set of 21 manuals (AA 001 009-001 029) used in APEX (Air Pollution Exercise), a computerized college and professional level "real world" game simulation of a community with urban and rural problems, industrial activities, and air pollution difficulties. For the purposes of the gaming exercise, APEX…

Instrumental neutron activation analysis for the certification of biological reference materials

International Nuclear Information System (INIS)

Ambulkar, M.N.; Chutke, N.L.; Garg, A.N.

1992-01-01

A multielemental instrumental neutron activation analysis (INAA) method by short and long irradiation has been employed for the determination of 22 minor and trace constituents in two proposed Standard Reference Materials P-RBF and P-WBF from Institute of Radioecology and Applied Nuclear Techniques, Czechoslovakia. Also some biological standards such as Bowen's Kale, Cabbage leaves (Poland) including wheat and rice flour samples of local origin were analysed. It is suggested that INAA is an ideal method for the certification of reference materials of biological matrices. (author). 7 refs., 1 tab

Survey of currently available reference materials for use in connection with the determination of trace elements in biological materials

International Nuclear Information System (INIS)

Parr, R.M.

1983-09-01

Elemental analysis of biological materials is at present the subject of intensive study by many different research groups throughout the world, in view of the importance of these trace elements in health and medical diagnosis. IAEA and other organizations are now making a variety of suitable reference materials available for use in connection with the determination of trace elements in biological materials. To help analysts in making a selection from among these various materials, the present report provides a brief survey of data for all such biological reference materials known to the author. These data are compiled by the author from January 1982 to June 1983

High-precision isotopic characterization of USGS reference materials by TIMS and MC-ICP-MS

Science.gov (United States)

Weis, Dominique; Kieffer, Bruno; Maerschalk, Claude; Barling, Jane; de Jong, Jeroen; Williams, Gwen A.; Hanano, Diane; Pretorius, Wilma; Mattielli, Nadine; Scoates, James S.; Goolaerts, Arnaud; Friedman, Richard M.; Mahoney, J. Brian

2006-08-01

The Pacific Centre for Isotopic and Geochemical Research (PCIGR) at the University of British Columbia has undertaken a systematic analysis of the isotopic (Sr, Nd, and Pb) compositions and concentrations of a broad compositional range of U.S. Geological Survey (USGS) reference materials, including basalt (BCR-1, 2; BHVO-1, 2), andesite (AGV-1, 2), rhyolite (RGM-1, 2), syenite (STM-1, 2), granodiorite (GSP-2), and granite (G-2, 3). USGS rock reference materials are geochemically well characterized, but there is neither a systematic methodology nor a database for radiogenic isotopic compositions, even for the widely used BCR-1. This investigation represents the first comprehensive, systematic analysis of the isotopic composition and concentration of USGS reference materials and provides an important database for the isotopic community. In addition, the range of equipment at the PCIGR, including a Nu Instruments Plasma MC-ICP-MS, a Thermo Finnigan Triton TIMS, and a Thermo Finnigan Element2 HR-ICP-MS, permits an assessment and comparison of the precision and accuracy of isotopic analyses determined by both the TIMS and MC-ICP-MS methods (e.g., Nd isotopic compositions). For each of the reference materials, 5 to 10 complete replicate analyses provide coherent isotopic results, all with external precision below 30 ppm (2 SD) for Sr and Nd isotopic compositions (27 and 24 ppm for TIMS and MC-ICP-MS, respectively). Our results also show that the first- and second-generation USGS reference materials have homogeneous Sr and Nd isotopic compositions. Nd isotopic compositions by MC-ICP-MS and TIMS agree to within 15 ppm for all reference materials. Interlaboratory MC-ICP-MS comparisons show excellent agreement for Pb isotopic compositions; however, the reproducibility is not as good as for Sr and Nd. A careful, sequential leaching experiment of three first- and second-generation reference materials (BCR, BHVO, AGV) indicates that the heterogeneity in Pb isotopic compositions

Quality of Standard Reference Materials for Short Time Activation Analysis

International Nuclear Information System (INIS)

Ismail, S.S.; Oberleitner, W.

2003-01-01

Some environmental reference materials (CFA-1633 b, IAEA-SL-1, SARM-1,BCR-176, Coal-1635, IAEA-SL-3, BCR-146, and SRAM-5) were analysed by short-time activation analysis. The results show that these materials can be classified in three groups, according to their activities after irradiation. The obtained results were compared in order to create a quality index for determination of short-lived nuclides at high count rates. It was found that Cfta is not a suitable standard for determining very short-lived nuclides (half-lives<1 min) because the activity it produces is 15-fold higher than that SL-3. Biological reference materials, such as SRM-1571, SRM-1573, SRM-1575, SRM-1577, IAEA-392, and IAEA-393, were also investigated by a higher counting efficiency system. The quality of this system and its well-type detector for investigating short-lived nuclides was discussed

Element concentrations in candidate biological and environmental reference materials by k0-standardized INAA

International Nuclear Information System (INIS)

Freitas, M.C.

1993-01-01

K 0 -Based Neutron Activation Analysis (k 0 INAA) was used to analyze the candidate reference materials Apple Leaves and Peach Leaves, and Oriental Tobacco Leaves and Virginia Tobacco Leaves. Concentration values for 27 elements were measured. The accuracy was ascertained by analysis of two certified reference materials. NIST 1572 Citrus Leaves and 1573 Tomato Leaves. The homogeneity test of the IAEA Evernia prunastri candidate reference material in aliquots ≥ 100 mg is extended to the elements Sc, Cr, Fe, Co, Zn, Rb, Sb, Cs, Ba, Ce and Th. (orig.)

Survey of currently available reference materials for use in connection with the determination of trace elements in biological and environmental materials

International Nuclear Information System (INIS)

Muramatsu, Y.; Parr, R.M.

1985-12-01

This report focuses on analytical reference materials which have been developed for use in connection with the determination of toxic and essential trace elements in biomedical and health-related environmental samples. Data are reported on 60 biological and 40 environmental (non-biological) reference materials from 11 suppliers. Certified concentration values (or their equivalents) and non-certified concentration values (or information values) are presented in various tables which are intended to help the user select a reference material that matches as closely as possible (i.e. with respect to matrix type and concentration of the element of interest) the ''real'' samples that are to be analysed. These tables have been generated from a database characterized by the following parameters: total number of reference materials=100; total number of elements recorded=69; total number of concentration values recorded=1771. Also included in the report is information (where available) on the cost of each material, the unit weight or volume supplied, and the minimum weight of material recommended for analysis. (author)

A on-line method for the determination of lead and lead isotope ratios in fresh and saline waters by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Halicz, Ludwik; Lam, J.W.H.; McLaren, J.W.

1994-01-01

A previously reported on-line ICP-MS method for the determination of lead and other trace elements in seawater has been re-examined to determine its suitability for the determination of lead isotope ratios ( 206 Pb/ 207 Pb and 207 Pb/ 208 Pb) in fresh and saline natural waters. A detection limit of 0.9 ng/1 for total lead (for a 5 ml sample) was achieved. Precision of isotope ratio data was 0.2-0.3% RSD at a Pb concentration of 1 μg/l, and was still better than 2% at concentrations of only 10-40 ng/1 in seawater certified reference materials (CRMs). For all three natural water CRMs examined, measured precision was very close to the limit predicted by counting statistics. (Author)

Preparation and certification of a uranium isotope certified reference material JAERI-U5

International Nuclear Information System (INIS)

Tamura, Shuzo; Hashitani, Hiroshi

1982-06-01

The Committee on Analytical Chemistry of Nuclear Fuels and Reactor Materials, JAERI had planned to prepare a new reference material, JAERI-U5 for uranium isotopic measurement since 1978. The reference material is composed of 6 samples of different enrichment in the range of 0.2 to 4.5 wt. percents of 235 U. The preparation includes dissolution of raw materials, blending of solutions, precipitation of ammonium diuranate, drying and ignition to U 3 O 8 . A mass-spectrometric collaborative analysis was carried out by well-trained two laboratories in this country, JAERI and PNC. The certified values were decided from the result of the collaborative work. As the measurements were based on NBS SRM's, JAERI-U5 should be called tertiary standard. The materials are packed in bottles of low-potassium-content glass for a possible use in non-destructive gamma-rays spectrometry. The reference material has been distributing from JAERI with a price of yen 140,000 per set (6 samples of 2 g of each) since 1979. (author)

Catalogue of reference materials of interest to nuclear energy

International Nuclear Information System (INIS)

1974-12-01

A provisional list of available chemical, isotopic and trace elements reference materials of interest to nuclear energy has been established. Emphasis has been given to the substances containing uranium and plutonium. Certified values, sample sizes, prices and addresses of suppliers are indicated

Analysis of FDA in-house food reference materials with anticoincidence INAA

International Nuclear Information System (INIS)

Anderson, D.L.; Cunningham, W.C.

2013-01-01

In-house reference material (IRM) cocoa powder (CCP) has been in use at US Food and Drug Administration laboratories for about 15 years. A single lot of commercial material was originally characterized for 32 elements by several laboratories and five techniques. A unique approach for basis weight determination based upon ambient relative humidity was developed for CCP, eliminating the need for dry weight determinations. The CCP Reference Sheet is updated by incorporating new results approximately every 5 years. The last update occurred in 2006. As part of an effort to revalidate and update values for CCP, anticoincidence instrumental neutron activation analysis (INAA) was used to determine mass fractions for 16 of the originally characterized elements, as well as to provide information on 16 other elements. Results were in very good agreement with 2006 Reference Sheet values. A new candidate IRM, fresh-frozen swordfish (FFSF) powder, was produced by adding inorganic As, Cd, Cr, Hg, Pb, Sb, and Se to liquid nitrogen-frozen commercial swordfish filets which were then homogenized. Portions of FFSF were analyzed by INAA to provide mass fraction and homogeneity information for As, Cd, Cr, Hg, Sb, and Se as well as for eight other elements occurring naturally in the material. Non-homogeneities were ≤2.5 % for As, Br, Cd, and Cs, and ≤1.8 % for Cr, Hg, Rb, Sb, and Se. Certified reference materials DORM-3 Fish Protein powder and fresh-frozen SRM 1947 Lake Michigan Fish Tissue were analyzed as controls. (author)

Optimization of instrumental neutron activation analysis for the within-bottle homogeneity study of reference materials of marine origin

International Nuclear Information System (INIS)

Silva, Daniel Pereira da

2017-01-01

The use of reference materials has been increasing in chemical analysis laboratories as its use is important for measurement validation in analytical chemistry. Such materials are generally imported, which require high financial investments in order to acquire them, and therefore it impacts on the difficulty to many national laboratories to use reference materials in their chemical analysis routine. Certification of reference materials is a complex process that assumes that the user is given appropriate assigned values of the properties of interests in the material. In this process, the homogeneity of the material must be checked. In this study, the within-bottle homogeneity study for the elements K, Mg, Mn, Na and V was performed for two reference materials of marine origin: the mussel reference material produced at the Neutron Activation Laboratory (LAN) of IPEN - CNEN/SP and an oyster tissue reference material produced abroad. For this purpose, the elements were determined in subsamples with masses varying between 1 and 250 mg by Instrumental Neutron Activation Analysis (INAA) and minimum sample intakes were estimated, ranging from 0.015 g for Na in the mussel reference material to 0.100 g for V in the two reference materials. (author)

Recommended reference materials for realization of physicochemical properties density

CERN Document Server

Herington, E F G

1976-01-01

This book first presents the nomenclature and units used in the determination of densities of liquids and solids, followed by a general description of the apparatus and the methods used in the measurement of density, with particular reference to the pycnometric, hydrostatic weighing, magnetic float, and temperature flotation methods. The use of water as a density reference material is then explained, focusing on the isotopic composition of Standard Mean Ocean Water (SMOW) and the absolute density of SMOW as a function of temperature. Problems due to the effect of pressure and dissolved gases o

The calibration of XRF polyethylene reference materials with k 0-NAA and ICP-AES

International Nuclear Information System (INIS)

Swagten, Josefien; Bossus, Daniel; Vanwersch, Hanny

2006-01-01

Due to the lack of commercially available polyethylene reference materials for the calibration of X-ray fluorescence spectrometers (XRF), DSM Resolve, in cooperation with PANalytical, prepared and calibrated such a set of standards in 2005. The reference materials were prepared based on the addition of additives to virgin polyethylene. The mentioned additives are added to improve the performance of the polymers. The elements present in additives are tracers for the used additives. The reference materials contain the following elements: F, Na, Mg, Al, Si, P, S, Ca, Ti and Zn in the concentration range of 5 mg/kg for Ti, up to 600 mg/kg for Mg. The calibration of the reference materials, including a blank, was performed using inductively coupled plasma atomic emission spectrometry (ICP-AES) and Neutron Activation Analysis (k 0 -NAA). ICP-AES was used to determine the elements Na, Mg, Al, P, Ca, Ti and Zn whereas k 0 -NAA was used for F, Na, Mg, Al, Ca, Ti and Zn. Over the complete concentration range, a good agreement of the results was found between the both techniques. This project has shown that within DSM Resolve, it is possible to develop and to calibrate homogenous reference materials for XRF

ENAA of iodine in standard reference material lyophilized human urine

International Nuclear Information System (INIS)

Zhang Yongbao; Wang Ke; Wang Ganfeng

1997-01-01

The contents of iodine in two kinds of standard reference materials lyophilized human urine are determined by ENAA. The sensitivity of this method is ten times higher than that of TNAA, and the relative standard deviations of ten measurements are 2.9% and 3.3%, respectively. Two certificated reference samples are used for verification of the analysis. The analytical results are in agreement with the recommended values, and the relative error is less than 3%

Baseline Assessment of 25-Hydroxyvitamin D Reference Material and Proficiency Testing/External Quality Assurance Material Commutability: A Vitamin D Standardization Program Study.

Science.gov (United States)

Phinney, Karen W; Sempos, Christopher T; Tai, Susan S-C; Camara, Johanna E; Wise, Stephen A; Eckfeldt, John H; Hoofnagle, Andrew N; Carter, Graham D; Jones, Julia; Myers, Gary L; Durazo-Arvizu, Ramon; Miller, W Greg; Bachmann, Lorin M; Young, Ian S; Pettit, Juanita; Caldwell, Grahame; Liu, Andrew; Brooks, Stephen P J; Sarafin, Kurtis; Thamm, Michael; Mensink, Gert B M; Busch, Markus; Rabenberg, Martina; Cashman, Kevin D; Kiely, Mairead; Galvin, Karen; Zhang, Joy Y; Kinsella, Michael; Oh, Kyungwon; Lee, Sun-Wha; Jung, Chae L; Cox, Lorna; Goldberg, Gail; Guberg, Kate; Meadows, Sarah; Prentice, Ann; Tian, Lu; Brannon, Patsy M; Lucas, Robyn M; Crump, Peter M; Cavalier, Etienne; Merkel, Joyce; Betz, Joseph M

2017-09-01

The Vitamin D Standardization Program (VDSP) coordinated a study in 2012 to assess the commutability of reference materials and proficiency testing/external quality assurance materials for total 25-hydroxyvitamin D [25(OH)D] in human serum, the primary indicator of vitamin D status. A set of 50 single-donor serum samples as well as 17 reference and proficiency testing/external quality assessment materials were analyzed by participating laboratories that used either immunoassay or LC-MS methods for total 25(OH)D. The commutability test materials included National Institute of Standards and Technology Standard Reference Material 972a Vitamin D Metabolites in Human Serum as well as materials from the College of American Pathologists and the Vitamin D External Quality Assessment Scheme. Study protocols and data analysis procedures were in accordance with Clinical and Laboratory Standards Institute guidelines. The majority of the test materials were found to be commutable with the methods used in this commutability study. These results provide guidance for laboratories needing to choose appropriate reference materials and select proficiency or external quality assessment programs and will serve as a foundation for additional VDSP studies.

Preparation and characterization of a Perna perna (Linnaeus, 1758) mussel reference material

International Nuclear Information System (INIS)

Moreira, Edson Goncalves

2010-01-01

The use of certified reference materials in chemical analysis is an important requirement in quality assurance systems, as it allows the validation of analytical methods and the realization of the metrological traceability of results. Then, it is possible to obtain valid and comparable results not only in space, but also in time. In this study, all the steps for the preparation of a national mussel reference material were attained, from the collection of the bulk material to processing steps such as freeze-drying, grinding, bottling and sterilization. Internationally accepted principles were applied for the homogeneity and stability assessment of the material, using instrumental neutron activation analysis and atomic absorption spectrometry as analytical techniques. By means of a collaborative program with participation of Brazilian and foreign laboratories, the chemical characterization of the material was performed. Element content in the mass percentage to mg kg -1 range was determined for 47 elements and some radionuclides, naturally present in the material. With the application of suitable statistical treatment to the data, it was considered that the content of 11 of those elements may be certified: As, Ca, Cl, Co, K, Mg, Mn, Na, Se, Th and Zn. This study may be considered an important step in the national metrological development, as it shows that the production and characterization of biological reference materials, mussel in particular, is feasible in Brazil, as a tool for quality assurance of environmental and nutritional studies performed in the country. (author)

Use of an excess variance approach for the certification of reference materials by interlaboratory comparison

International Nuclear Information System (INIS)

Crozet, M.; Rigaux, C.; Roudil, D.; Tuffery, B.; Ruas, A.; Desenfant, M.

2014-01-01

In the nuclear field, the accuracy and comparability of analytical results are crucial to insure correct accountancy, good process control and safe operational conditions. All of these require reliable measurements based on reference materials whose certified values must be obtained by robust metrological approaches according to the requirements of ISO guides 34 and 35. The data processing of the characterization step is one of the key steps of a reference material production process. Among several methods, the use of interlaboratory comparison results for reference material certification is very common. The DerSimonian and Laird excess variance approach, described and implemented in this paper, is a simple and efficient method for the data processing of interlaboratory comparison results for reference material certification. By taking into account not only the laboratory uncertainties but also the spread of the individual results into the calculation of the weighted mean, this approach minimizes the risk to get biased certified values in the case where one or several laboratories either underestimate their measurement uncertainties or do not identify all measurement biases. This statistical method has been applied to a new CETAMA plutonium reference material certified by interlaboratory comparison and has been compared to the classical weighted mean approach described in ISO Guide 35. This paper shows the benefits of using an 'excess variance' approach for the certification of reference material by interlaboratory comparison. (authors)

Multielement comparison of instrumental neutron activation analysis techniques using reference materials

International Nuclear Information System (INIS)

Ratner, R.T.; Vernetson, W.G.

1995-01-01

Several instrumental neutron activation analysis techniques (parametric, comparative, and k o -standardization) are evaluated using three reference materials. Each technique is applied to National Institute of Standards and Technology standard reference materials, SRM 1577a (Bovine Liver) and SRM 2704 (Buffalo River Sediment), and the United States Geological Survey standard BHVO-1 (Hawaiian Basalt Rock). Identical (but not optimum) irradiation, decay, and counting schemes are employed with each technique to provide a basis for comparison and to determine sensitivities in a routine irradiation scheme. Fifty-one elements are used in this comparison; however, several elements are not detected in the reference materials due to rigid analytical conditions (e.g. insufficient length of irradiation or activity for radioisotope of interest decaying below the lower limit of detection before counting interval). Most elements are normally distributed around certified or consensus values with a standard deviation of 10%. For some elements, discrepancies are observed and discussed. The accuracy, precision, and sensitivity of each technique are discussed by comparing the analytical results to consensus values for the Hawaiian Basalt Rock to demonstrate the diversity of multielement applications. (author) 4 refs.; 2 tabs

Development of a certified reference materials for composition of citric acid

Directory of Open Access Journals (Sweden)

D. H. Kulev

2014-01-01

Full Text Available The paper presents a summary of analyzing Technical Regulations of the Customs Union TR TC 029/2012 "Safety Requirements for Food Additives, Flavorings and Technological Processing Aids". Information on certified reference materials (RMs for composition of citric acid is provided. Certified characteristics of the RM are, on the one hand, mass fraction of the base substance and, on the other hand, mass fraction of impurities - toxic elements (lead, arsenic, cadmium, mercury. The first batches of the given RMs are produced, which are registered in the State Register of the approved types of certified reference materials GS010300-2013 and GS010143-2012.

REFERENCE MATERIALS SYSTEM OF SCIENTIFIC METHODICAL CENTRE OF STATE SERVICE OF REFERENCE MATERIALS FOR COMPOSITION AND PROPERTIES OF SUBSTANCES AND MATERIALS URAL RESEARCH INSTITUTE FOR METROLOGY

Directory of Open Access Journals (Sweden)

E. V. Osinseva

2015-01-01

Full Text Available Since 1960s UNIIM performs research in the field of needs in reference materials of composition and properties of substances and materials (RM as well as develops it. During the research UNIIM has developed 757 types of RMs for metrological measurement assurance of factors of composition and properties of substance and materials for test laboratories of chemical, pharmaceutical, fuel, food industry, agriculture, metallurgy and ecological monitoring laboratories. List ofRMs enlarges thanks to development of UNIIM standards and transmission measurement facility from State standards of units. Taking into account the actual requirements in the field of measurements, the UNIIM's key destination is to assure the accuracy and the metrological traceability of measurements. The present-day system of RMs to be developed in UNIIM includes RMs of composition of inorganic and organic compounds and their solutions, fuels, stable isotopic materials, water, grounds, food products, biomaterials, nanomaterials, metals, alloys and other materials offerrous and non-ferrous industry, RMs of properties (thermodynamic, magnetic, physical-chemical, technical of substances and materials. The present article considers history of RMs list development which were created by UNIIM and the strategy of this direction.

Proposals for the use of reference materials and for the development of in-house quality control materials for food analysis

International Nuclear Information System (INIS)

Ihnat, Milan

2002-01-01

A summary is presented of factors to be considered in the development of food-based in-house quality control materials to augment available Reference Materials and for frequent, concerted data quality control. Some guidelines are offered regarding approaches to the many considerations required for such an endeavour. Preliminary draft recommendations containing a sequence of steps has been compiled as a starting proposal for a food quality control material development scheme, for a range of natural matrices and measurands. In addition, information on the selection and utilization of Certified Reference Materials and procedures for performance interpretation and corrective action is provided. (author)

A candidate liquid chromatography mass spectrometry reference method for the quantification of the cardiac marker 1-32 B-type natriuretic peptide.

Science.gov (United States)

Torma, Attila F; Groves, Kate; Biesenbruch, Sabine; Mussell, Chris; Reid, Alan; Ellison, Steve; Cramer, Rainer; Quaglia, Milena

2017-08-28

B-type natriuretic peptide (BNP) is a 32 amino acid cardiac hormone routinely measured by immunoassays to diagnose heart failure. While it is reported that immunoassay results can vary up to 45%, no attempt of standardization and/or harmonization through the development of certified reference materials (CRMs) or reference measurement procedures (RMPs) has yet been carried out. B-type natriuretic peptide primary calibrator was quantified traceably to the International System of Units (SI) by both amino acid analysis and tryptic digestion. A method for the stabilization of BNP in plasma followed by protein precipitation, solid phase extraction (SPE) and liquid chromatography (LC) mass spectrometry (MS) was then developed and validated for the quantification of BNP at clinically relevant concentrations (15-150 fmol/g). The candidate reference method was applied to the quantification of BNP in a number of samples from the UK NEQAS Cardiac Markers Scheme to demonstrate its applicability to generate reference values and to preliminary evaluate the commutability of a potential CRM. The results from the reference method were consistently lower than the immunoassay results and discrepancy between the immunoassays was observed confirming previous data. The application of the liquid chromatography-mass spectrometry (LC-MS) method to the UK NEQAS samples and the correlation of the results with the immunoassay results shows the potential of the method to support external quality assessment schemes, to improve understanding of the bias of the assays and to establish RMPs for BNP measurements. Furthermore, the method has the potential to be multiplexed for monitoring circulating truncated forms of BNP.

Measurement of polybrominated diphenyl ethers in environmental matrix standard reference materials

Energy Technology Data Exchange (ETDEWEB)

Stapleton, H.; Schantz, M.; Wise, S. (National Institute of Standards and Technology)

2004-09-15

Polybrominated diphenyl ethers (PBDEs) are a class of emerging contaminants of concern as many studies have now demonstrated that these compounds are bioaccumulative, persistent and increasing in concentration in the environment. PBDEs are being detected in almost every environmental sample examined, and they have even been measured in samples collected in the Arctic, further demonstrating their persistence and potential for long range transport. More and more studies are continuing to examine the fate and transport of these flame retardant compounds in environmental samples and as such, reference materials are needed to provide quality control on these measurements. The National Institute of Standards and Technology (NIST) supports a national Standard Reference Material (SRM) program for measurement of organic contaminants such as PCBs, PAHs and chlorinated pesticides in environmental matrices. This current study was undertaken to provide reference measurements for PBDEs in selected SRMs that are currently used by various laboratories throughout the United States. These SRMs include matrices such as marine mammal blubber, lake trout tissue, mussel tissue, sediment, house dust and human serum. We report here reference values for 22 PBDE congeners that have been quantified in these seven types of SRMs.

IRMM Certified Reference Materials and k0-NAA: an important role for the future

International Nuclear Information System (INIS)

Robouch, P.; Arana, G.; Pauwels, J.; Pomm, S.

1998-01-01

The k 0 -Neutron Activation Analysis method was introduced at the Institute for Reference Materials and Measurements (IRMM) and the Belgian nuclear research centre (SCK CEN) in 1994. This analytical technique is routinely used at IRMM for the production control, homogeneity and stability tests and/or for certification of metallic, biological and environmental reference materials. The successful implementation of k 0 -NAA was proven at several certification exercises - such as ISS Antarctic Sediment, BCR Mussel Tissue and BCR Bovine Liver, SMU Bovine Blood - where all our results were accepted for certification. Responding to regulatory and/or scientific demands, IRMM is collaborating with national institutes to develop new high quality reference materials: (i) in the field of Neutron dosimetry: high purity nickel, Al-Ag or Zr-Au-Lu alloys; (ii) for environmental and industrial monitoring: Antarctic krill, doped plastics or catalytic converters; (iii) synthetic multi-element standard for the accreditation of k 0 -NAA laboratories. Far from being exhaustive, this list highlights the important role that k 0 -NAA will play in the certification of reference materials in the years 2000. (author)

Reference material certification of chinese cabbage composition for selenium, nitrogen, phosphorus and potassium content

Directory of Open Access Journals (Sweden)

D. A. Chupakhin

2016-01-01

Full Text Available Rationale. The reference material of composition with the established metrological characteristics including a certified value and an expanded uncertainty is necessary to ensure an effective accuracy and precision control of results of element composition determination in food ingredients and products. This paper represents the development of a reference material of food crop composition for selenium, nitrogen, phosphorus and potassium content. Methods. To identify the selenium the hybrid atomic absorption method was used, to identify the nitrogen and phosphorus the photometric method was used, to determine the potassium flame-photometric method was used. When determining the metrological characteristics of the reference material the Russian national instructions and recommendations MI 3174-2009 and P 50.2.058-2007 were applied. Results. Based on the research findings the reference material of Chinese cabbage composition with a certified value and an expanded uncertainty was developed: for selenium 0.044 ± 0.017 mg/kg; for nitrogen 4.09 ± 0.27 %; for phosphorus 0.69 ± 0.14 %; for potassium 2.87 ± 0.22 %.

Multicenter evaluation of the commutability of a potential reference material for harmonization of enzyme activities

NARCIS (Netherlands)

Scharnhorst, V.; Apperloo, J.J.; Baadenhuijsen, H.; Vader, H.L.

2014-01-01

Standardization of laboratory results allows for the use of common reference intervals and can be achieved via calibration of field methods with secondary reference materials. These harmonization materials should be commutable, i.e., they produce identical numerical results independent of assay

Interlaboratory Reproducibility of Droplet Digital Polymerase Chain Reaction Using a New DNA Reference Material Format.

Science.gov (United States)

Pinheiro, Leonardo B; O'Brien, Helen; Druce, Julian; Do, Hongdo; Kay, Pippa; Daniels, Marissa; You, Jingjing; Burke, Daniel; Griffiths, Kate; Emslie, Kerry R

2017-11-07

Use of droplet digital PCR technology (ddPCR) is expanding rapidly in the diversity of applications and number of users around the world. Access to relatively simple and affordable commercial ddPCR technology has attracted wide interest in use of this technology as a molecular diagnostic tool. For ddPCR to effectively transition to a molecular diagnostic setting requires processes for method validation and verification and demonstration of reproducible instrument performance. In this study, we describe the development and characterization of a DNA reference material (NMI NA008 High GC reference material) comprising a challenging methylated GC-rich DNA template under a novel 96-well microplate format. A scalable process using high precision acoustic dispensing technology was validated to produce the DNA reference material with a certified reference value expressed in amount of DNA molecules per well. An interlaboratory study, conducted using blinded NA008 High GC reference material to assess reproducibility among seven independent laboratories demonstrated less than 4.5% reproducibility relative standard deviation. With the exclusion of one laboratory, laboratories had appropriate technical competency, fully functional instrumentation, and suitable reagents to perform accurate ddPCR based DNA quantification measurements at the time of the study. The study results confirmed that NA008 High GC reference material is fit for the purpose of being used for quality control of ddPCR systems, consumables, instrumentation, and workflow.

Present status and future plans of the study for preparation of Pu reference materials

International Nuclear Information System (INIS)

Sumi, Mika; Kageyama, Tomio; Suzuki, Toru

2007-01-01

All accountancy analysis at the Plutonium Fuel Development Center of JAEA is performed by isotope dilution mass spectrometry with well-characterized standard materials. Though Pu reference materials has been supplied from foreign country, importing those Pu materials is gradually becoming more difficult and may be almost impossible to import them in future. Thus, in order to establish the capability and expertise for the preparation of Pu reference materials, JAEA has started collaborative work with NBL who has high skills for preparing and supplying nuclear reference materials for long periods. One of the targets of this collaboration is preparation of standard material for IDMS (LSD spike). MOX powder which has been stored in JAEA was dissolved and Purified to obtain Pu solution. A small portion of the Purified solution was transported to NBL for analysis. LSD spike will be prepared from this Pu solution and then validation analysis and performance test including stability test will be performed with NBL and JAEA. This report presents status and future plans for the collaboration work. (author)

Certified Reference Materials for Radioactivity Measurements in Environmental Samples of Soil and Water: IAEA-444 and IAEA-445

International Nuclear Information System (INIS)

2011-01-01

Reference Materials are an important requirement for any sort of quantitative chemical and radiochemical analysis. Laboratories need them for calibration and quality control throughout their analytical work. The IAEA started to produce reference materials in the early 1960's to meet the needs of the analytical laboratories in its Member States that required reference materials for quality control of their measurements. The initial efforts were focused on the preparation of environmental reference materials containing anthropogenic radionuclides for use by those laboratories employing nuclear analytical techniques. These reference materials were characterized for their radionuclide content through interlaboratory comparison involving a core group of some 10 to 20 specialist laboratories. The success of these early exercises led the IAEA to extend its activities to encompass both terrestrial and marine reference materials containing primordial radionuclides and trace elements. Within the frame of IAEA activities in production and certification of reference materials, this report describes the certification of the IAEA-444 and IAEA-445: soil and water spiked with gamma emitting radionuclides respectively. Details are given on methodologies and data evaluation

Development of Lentivirus-Based Reference Materials for Ebola Virus Nucleic Acid Amplification Technology-Based Assays.

Science.gov (United States)

Mattiuzzo, Giada; Ashall, James; Doris, Kathryn S; MacLellan-Gibson, Kirsty; Nicolson, Carolyn; Wilkinson, Dianna E; Harvey, Ruth; Almond, Neil; Anderson, Robert; Efstathiou, Stacey; Minor, Philip D; Page, Mark

2015-01-01

The 2013-present Ebola virus outbreak in Western Africa has prompted the production of many diagnostic assays, mostly based on nucleic acid amplification technologies (NAT). The calibration and performance assessment of established assays and those under evaluation requires reference materials that can be used in parallel with the clinical sample to standardise or control for every step of the procedure, from extraction to the final qualitative/quantitative result. We have developed safe and stable Ebola virus RNA reference materials by encapsidating anti sense viral RNA into HIV-1-like particles. The lentiviral particles are replication-deficient and non-infectious due to the lack of HIV-1 genes and Envelope protein. Ebola virus genes were subcloned for encapsidation into two lentiviral preparations, one containing NP-VP35-GP and the other VP40 and L RNA. Each reference material was formulated as a high-titre standard for use as a calibrator for secondary or internal standards, and a 10,000-fold lower titre preparation to serve as an in-run control. The preparations have been freeze-dried to maximise stability. These HIV-Ebola virus RNA reference materials were suitable for use with in-house and commercial quantitative RT-PCR assays and with digital RT-PCR. The HIV-Ebola virus RNA reference materials are stable at up to 37°C for two weeks, allowing the shipment of the material worldwide at ambient temperature. These results support further evaluation of the HIV-Ebola virus RNA reference materials as part of an International collaborative study for the establishment of the 1st International Standard for Ebola virus RNA.

Development of Lentivirus-Based Reference Materials for Ebola Virus Nucleic Acid Amplification Technology-Based Assays.

Directory of Open Access Journals (Sweden)

Giada Mattiuzzo

Full Text Available The 2013-present Ebola virus outbreak in Western Africa has prompted the production of many diagnostic assays, mostly based on nucleic acid amplification technologies (NAT. The calibration and performance assessment of established assays and those under evaluation requires reference materials that can be used in parallel with the clinical sample to standardise or control for every step of the procedure, from extraction to the final qualitative/quantitative result. We have developed safe and stable Ebola virus RNA reference materials by encapsidating anti sense viral RNA into HIV-1-like particles. The lentiviral particles are replication-deficient and non-infectious due to the lack of HIV-1 genes and Envelope protein. Ebola virus genes were subcloned for encapsidation into two lentiviral preparations, one containing NP-VP35-GP and the other VP40 and L RNA. Each reference material was formulated as a high-titre standard for use as a calibrator for secondary or internal standards, and a 10,000-fold lower titre preparation to serve as an in-run control. The preparations have been freeze-dried to maximise stability. These HIV-Ebola virus RNA reference materials were suitable for use with in-house and commercial quantitative RT-PCR assays and with digital RT-PCR. The HIV-Ebola virus RNA reference materials are stable at up to 37°C for two weeks, allowing the shipment of the material worldwide at ambient temperature. These results support further evaluation of the HIV-Ebola virus RNA reference materials as part of an International collaborative study for the establishment of the 1st International Standard for Ebola virus RNA.

Accuracy and Precision in Elemental Analysis of Environmental Samples using Inductively Coupled Plasma-Atomic Emission Spectrometry

International Nuclear Information System (INIS)

Quraishi, Shamsad Begum; Chung, Yong-Sam; Choi, Kwang Soon

2005-01-01

Inductively Coupled Plasma-Atomic Emission Spectrometry followed by micro-wave digestion have been performed on different environmental Certified Reference Materials (CRMs). Analytical results show that accuracy and precision in ICP-AES analysis were acceptable and satisfactory in case of soil and hair CRM samples. The relative error of most of the elements in these two CRMs is within 10% with few exceptions and coefficient of variation is also less than 10%. Z-score as an analytical performance was also within the acceptable range (±2). ICP-AES was found as an inadequate method for Air Filter CRM due to incomplete dissolution, low concentration of elements and very low mass of the sample. However, real air filter sample could have been analyzed with high accuracy and precision by increasing sample mass during collection. (author)

Two spruce shoot candidate reference materials from the German environmental specimen bank

International Nuclear Information System (INIS)

Backhaus, F.; Bagschik, U.; Burow, M.; Froning, M.; Mohl, C.; Ostapczuk, P.; Rossbach, M.; Schladot, J.D.; Stoeppler, M.; Waidmann, E.; Byrne, A.R.; Zeisler, R.

1994-01-01

Two new materials are introduced that might serve as useful aids for the harmonisation of analytical results. Spruce shoots, cryogenically homogenized and characterized for 50 elements from two sampling sites of the German Environmental Specimen Bank (ESB) are presented as possible third generation reference materials that might also act as calibrating materials in speciation analysis. (author)

Certified reference material IAEA-418: I-129 in Mediterranean sea water

International Nuclear Information System (INIS)

2009-01-01

Our society is attaching increasing importance to the study and assessment of the state and health of the environment. Organizations involved in such activities rely on the quality of the information provided and, ultimately, on the precision and accuracy of the data on which the information is based. Many laboratories are involved in the production of environmental data in many cases leading to wider assessments. These laboratories may develop and validate new analytical methods, study the environmental impact of human activities, provide services to other organizations, etc. In particular, laboratories are providing data on levels of radioactivity in a variety of marine matrixes such as water, suspended matter, sediments and biota. Because of the need to base scientific conclusions on valid and internationally comparable data, the need to provide policy makers with correct information and the need for society to be informed of the state of the environment, it is indispensable to ensure the quality of the data produced by each laboratory. Principles of good laboratory practice require both internal and external procedures to verify the quality of the data produced. Internal quality is verified in a number of ways such as the use of laboratory information systems, keeping full records of equipment performance and standardization of analytical procedures. External quality can also be ascertained in a number of ways, notably accreditation by an external body under a defined quality scheme but also, amongst others, the use of internationally accepted calibration standards that are traceable to the SI international system of units, the participation in interlaboratory comparisons or the regular use of reference materials to test laboratory performance. The Radiometrics Laboratory of the IAEA Marine Environment Laboratories has been providing quality products for the last 40 years which include the organization of interlaboratory comparisons, proficiency tests

Elaboration and characterisation of plutonium waste reference materials

International Nuclear Information System (INIS)

Perolat, J.P.

1990-01-01

The Analysis Methods Establishment Commission (CETAMA) has set up a program for the elaboration and characterisation of plutonium waste reference materials. The object of this program is to give laboratories the possibility to test and calibrate apparatus used in non-destructive methods for the analysis of plutonium waste. The different parameters of this program are presented: - characterisation of plutonium, - type and number of containers, - plutonium distribution inside the different containers, - description of the matrix

INAA and flame AAS of various vegetable reference materials

International Nuclear Information System (INIS)

Djingova, R.; Arpadjan, S.; Kuleff, I.

1991-01-01

INAA and flame AAS have been used for the analysis of a large number of vegetable reference materials. Out of all determined elements (28 by INAA and 11 by AAS) nine are common for both methods (Ca, Cd, Co, Cu, Fe, Mg, Mn, Na, Zn) and for these the possibilities of the two methods have been compared. (orig.)

Characterization of Ricin and R. communis Agglutinin Reference Materials

Science.gov (United States)

Worbs, Sylvia; Skiba, Martin; Söderström, Martin; Rapinoja, Marja-Leena; Zeleny, Reinhard; Russmann, Heiko; Schimmel, Heinz; Vanninen, Paula; Fredriksson, Sten-Åke; Dorner, Brigitte G.

2015-01-01

Ricinus communis intoxications have been known for centuries and were attributed to the toxic protein ricin. Due to its toxicity, availability, ease of preparation, and the lack of medical countermeasures, ricin attracted interest as a potential biological warfare agent. While different technologies for ricin analysis have been established, hardly any universally agreed-upon “gold standards” are available. Expert laboratories currently use differently purified in-house materials, making any comparison of accuracy and sensitivity of different methods nearly impossible. Technically challenging is the discrimination of ricin from R. communis agglutinin (RCA120), a less toxic but highly homologous protein also contained in R. communis. Here, we established both highly pure ricin and RCA120 reference materials which were extensively characterized by gel electrophoresis, liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI MS/MS), and matrix-assisted laser desorption ionization–time of flight approaches as well as immunological and functional techniques. Purity reached >97% for ricin and >99% for RCA120. Different isoforms of ricin and RCA120 were identified unambiguously and distinguished by LC-ESI MS/MS. In terms of function, a real-time cytotoxicity assay showed that ricin is approximately 300-fold more toxic than RCA120. The highly pure ricin and RCA120 reference materials were used to conduct an international proficiency test. PMID:26703723

Characterization of Ricin and R. communis Agglutinin Reference Materials

Directory of Open Access Journals (Sweden)

Sylvia Worbs

2015-11-01

Full Text Available Ricinus communis intoxications have been known for centuries and were attributed to the toxic protein ricin. Due to its toxicity, availability, ease of preparation, and the lack of medical countermeasures, ricin attracted interest as a potential biological warfare agent. While different technologies for ricin analysis have been established, hardly any universally agreed-upon “gold standards” are available. Expert laboratories currently use differently purified in-house materials, making any comparison of accuracy and sensitivity of different methods nearly impossible. Technically challenging is the discrimination of ricin from R. communis agglutinin (RCA120, a less toxic but highly homologous protein also contained in R. communis. Here, we established both highly pure ricin and RCA120 reference materials which were extensively characterized by gel electrophoresis, liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI MS/MS, and matrix-assisted laser desorption ionization–time of flight approaches as well as immunological and functional techniques. Purity reached >97% for ricin and >99% for RCA120. Different isoforms of ricin and RCA120 were identified unambiguously and distinguished by LC-ESI MS/MS. In terms of function, a real-time cytotoxicity assay showed that ricin is approximately 300-fold more toxic than RCA120. The highly pure ricin and RCA120 reference materials were used to conduct an international proficiency test.

Contribution of NAA and other techniques to the certification of two new Polish CRMs prepared by INCT

International Nuclear Information System (INIS)

Dybczynski, R.; Danko, B.; Kulisa, K.; Maleszewska, E.; Polkowska-Motrenko, H.; Samczynski, Z.; Szopa, Z.

2002-01-01

Two new reference materials of biological origin, namely Tea Leaves (INCTTL-1 ) and Mixed Polish Herbs (INCT-MPH-2), were prepared, and a worldwide interlaboratory comparison in which more than 100 laboratories participated was organized with the aim to certify these materials for the content of possibly a great number of trace elements. In this paper a preliminary analysis of the contribution of various analytical techniques to the certification of the new reference materials is presented and discussed with special emphasis on the role played by neutron activation analysis (NAA) and other radiometric techniques. The significance of 'very accurate methods' by radiochemical NAA in the certification process is pointed out. An attempt is made to compare the outcome of the present intercomparison with those formerly organized by INCT as well as with some earlier IAEA intercomparisons in order to demonstrate similarities, differences and trends in the use of the various analytical techniques in trace analysis as a function of time. (author)

Certification of a meat reference material based on a collaborative study

Directory of Open Access Journals (Sweden)

Claudia Marcela Salazar Arzate

2013-01-01

Full Text Available Through a collaborative project, comparison studies were carried out to improve measurement capabilities of participating laboratories, supporting them to produce, characterize and distribute reference materials in the food sector. The project was planned in four annual stages (milk, water, meat and grains. The third stage aimed specifically to quantify and certify the nutritional content of the parameters (nitrogen, fat, sodium and potassium of a batch candidate as Certified Reference Material (CRM of canned beef. This study was conducted in collaboration between several National Metrology Institutes (NMIs and/or collaborating laboratories, which, once identified the possible causes of variability or bias in the measurements, as well as the opportunities of improvement, achieved the certification of the material beef. The CRM was distributed among the participants to cover the needs of the food industry of meat products and testing laboratories in their respective countries.

Determination of multielement in optical waveguide and standard reference materials by instrumental neutron activation analysis

International Nuclear Information System (INIS)

Kobayashi, K.; Kudo, K.

1979-01-01

Trace amounts of transition elements (Co, Cr, Cu, Fe, Mn and V) and other seven elements in optical waveguide samples were determined by INAA. The contents of impurities in ultre-pure materials are less than those of high-purity materials and of G.R. grade. The increase of contamination of trace transition elements and iridium from furnace or crucible are observed in the production of optical glass fibers. Up to seventeen elements were determined in five NBS biological standard reference materials: Oyster Tissue: SRM-1566, Brewers Yeast: SRM-1569, Spinach: SRM-1570, Orchard Leaves: SRM-1571 and Tuna Fish, and in four Japanese biological standard reference materials: Tea Leaves B and C, Pepperbush and Shark Meat. The analytical results in NBS and Japanese standard reference materials are in good agreement with published values and certified values by NBS. (author)

Thallium determination in reference materials by isotope dilution mass spectrometry (IDMS) using thermal ionization

International Nuclear Information System (INIS)

Waidmann, E.; Hilpert, K.; Stoeppler, M.

1990-01-01

Using Isotope Dilution Mass Spectrometry (IDMS) with thermal ionization, thallium concentrations were determined in reference materials from NIST and BCR, from other sources, and reference materials from the German Environmental Specimen Bank 203 Tl spike solution is applied for the isotope dilution technique. Thallium concentrations in the investigated materials range from 2.67 μg Tl.kg -1 to 963 μg Tl.kg -1 with a relative standard deviation from 0.14 to 10%. The detection limit was 0.1 ng thallium for this work. (orig.)

The preparation and analysis of minerals for use as reference material

International Nuclear Information System (INIS)

Stoch, H.

1976-01-01

This report covers the progress made in the collection of the material for reference samples, and the five interlaboratory analytical programmes (ferrochromium slags, fluorspar, 'mixed' NIMROC samples, rare earths, and ferromanganese slags). The description of the internal analytical programme has been subdivided into eight main categories, and a comprehensive list of evaluated results covering a wide range of materials is included. Additional results for thorium, rare earths, tin, tantalum, and niobium for the appropriate reference samples are included in updated tables. The main purpose in the preparation of these samples is to provide control samples for analytical work at the National Institute for Metallurgy. Where there is a special need, limited quantities of the samples can be made available to other laboratories

Analysis of marine sediment and lobster hepatopancreas reference materials by instrumental photon activation

International Nuclear Information System (INIS)

Landsberger, S.; Davidson, W.F.

1985-01-01

By use of instrumental photon activation analysis, twelve trace (As, Ba, Cr, Co, Mn, Ni, Pb, Sb, Sr, U, Zn, and Zr) and eight minor (C, Na, Mg, Co, K, Ca, Tl, and Fe) elements were determined in a certified marine sediment standard reference material as well as eight trace (Mn, Ni, Cu, Zn, As, Sr, Cd, and Pb) and four minor (Na, Mg, Cl, and Ca) elements in a certified marine tissue (lobster hepatopancreas) standard reference material. The precision and accuracy of the present results when compared to the accepted values clearly demonstrate the reliability of this nondestructive technique and its applicability to marine environmental or marine geochemical studies. 24 references, 4 figures, 3 tables

Bronze analysis by k0-NAA and PIXE

International Nuclear Information System (INIS)

Arana, G.; Waetjen, U.; Ingelbrecht, C.; Robouch, P.

2003-01-01

Five copper alloys were prepared with modern powder metallurgical processes in the frame of the European project 'Improvement of Means of Measurement on Archaeological Copper-Alloys for Characterisation and Conservation (IMMACO)' and certified for As, Pb, Sn and Zn mass fractions. Similar in their composition to archaeological bronze alloys, these Certified Reference Materials (CRMs) are to be used for calibration of XRF instruments for characterization of archaeological samples either in the laboratory or in the field. Successful contribution of non-destructive analytical methods (k 0 -NAA and PIXE) to the IMMACO project and to the certification of the five reference materials is presented. (author)

Evaluation of botanical reference materials for the determination of vanadium in biological samples

International Nuclear Information System (INIS)

Heydorn, K.; Damsgaard, E.

1982-01-01

Three botanical reference materials prepared by the National Bureau of Standards have been studied by neutron activation analysis to evaluate their suitability with respect to the determination of vanadium in biological samples. Various decomposition methods were applied in connection with chemical or radiochemical separations, and results for vanadium were compared with those found by purely instrumental neutron activation analysis. Significantly lower results indicate losses or incomplete dissolution, which makes SRM 1575 Pine Needles and SRM 1573 Tomato Leaves less satisfactory than SRM 1570 Spinach. A reference value of 1.15 mg/kg of this material is recommended, based on results from 3 different methods. All three materials are preferable to SRM 1571 Orchard Leaves, while Bowen's Kale remains the material of choice because of its lower concentration. (author)

Determination of sampling constants in NBS geochemical standard reference materials

International Nuclear Information System (INIS)

Filby, R.H.; Bragg, A.E.; Grimm, C.A.

1986-01-01

Recently Filby et al. showed that, for several elements, National Bureau of Standards (NBS) Fly Ash standard reference material (SRM) 1633a was a suitable reference material for microanalysis (sample weights 2 , and the mean sample weight, W vector, K/sub s/ = (S/sub s/%) 2 W vector, could not be determined from these data because it was not possible to quantitate other sources of error in the experimental variances. K/sub s/ values for certified elements in geochemical SRMs provide important homogeneity information for microanalysis. For mineralogically homogeneous SRMs (i.e., small K/sub s/ values for associated elements) such as the proposed clays, it is necessary to determine K/sub s/ by analysis of very small sample aliquots to maximize the subsampling variance relative to other sources of error. This source of error and the blank correction for the sample container can be eliminated by determining K/sub s/ from radionuclide activities of weighed subsamples of a preirradiated SRM

Reference Material IAEA 434: Naturally Occurring Radionuclides in Phosphogypsum

International Nuclear Information System (INIS)

2010-01-01

Phosphogypsum is generated as a by-product of the phosphoric acid based fertilizer industry. The discharge of phosphogypsum on earth surface deposits is a potential source of enhanced natural radiation and heavy metals, and the resulting environmental impact should be considered carefully to ensure safety and compliance with environmental regulations. In addition, phosphogypsum can be used to make several building materials and it is used in agriculture as a conditioner to maintain soil productivity in areas where soils are poor and erode easily. A reliable determination of naturally occurring radionuclides in phosphogypsum is necessary to comply with the radiation protection and environmental regulations. The IAEA-434 will assist laboratories in the IAEA Member States in validating their analytical methods for the determination of naturally occurring radionuclides in phosphogypsum and to control the quality of the produced analytical results. Reference values for the massic activities and associated standard uncertainties were established for: Pb-210, Ra-226, Th-230, U-234 and U-238. During sample production and certification, the requirements for reference material production and certification as stated in ISO guides 34 and 35 were taken into account. This report summarizes the preparation and certification process

Feasibility Study for the Development of Plutonium Reference Materials for Age Dating in Nuclear Forensics

International Nuclear Information System (INIS)

Sturm, M.; Richter, S.; Aregbe, Y.; Wellum, R.; Altzitzoglou, T.; Verbruggen, A.; Mayer, K.; Prohaska, T.

2010-01-01

Isotopic reference materials certified for the age of nuclear material (uranium, plutonium) are needed in the fields of nuclear forensics and environmental measurements. Therefore a feasibility study for the development of plutonium reference materials for age dating has been started recently at the Institute for Reference Materials and Measurements (EC-JRC-IRMM). The ''age'' of the material is defined as the time that has passed since the last chemical separation of the mother and daughter isotopes (e.g. 241 Pu and 241 Am). Assuming that the separation has been complete and all the daughter isotopes have been removed from the original material during this last separation, the age of the material can be determined by measuring the ratio of daughter and mother radio-nuclides, e.g. 241 Am/ 241 Pu. At a given time after the last separation and depending on the half lives of the radio-nuclides involved, a certain amount of the daughter radionuclide(s) will be present. For the determination of the unknown age of a material different ''clocks'' can be used; ''clocks'' are pairs of mother and daughter radio-nuclides, such as 241 Am/ 241 Pu, 238 Pu/ 234 U, 239 Pu/ 235 U, 240 Pu/ 236 U, and possibly 242 Pu/ 238 U. For the age estimation of a real sample, such as material seized in nuclear forensics investigations or dust samples in environmental measurements, it is advisable to use more than one clock in order to ensure the reliability of the results and to exclude the possibility that the sample under question is a mixture of two or more materials. Consequently, a future reference material certified for separation date should ideally be certified for more than one ''clock'' or several reference materials for different ''clocks'' should be developed. The first step of this study is to verify the known separation dates of different plutonium materials of different ages and isotopic compositions by measuring the mother ( 238 Pu, 239 Pu, 240 Pu, 241 Pu, 242 Pu) and daughter

Report of the research co-ordination meeting on reference materials for microanalytical nuclear techniques

International Nuclear Information System (INIS)

1994-01-01

Many microanalytical procedure require specific natural-matrix reference materials containing very low levels of trace elements and having a high degree of homogeneity. This proposed CRP will specifically address the question of quality control materials for these techniques. The participants of the meeting discussed the requirements for certified reference materials to by used in microanalysis with particular emphasis on the homogeneity issues. This publication contains summary of the discussions along with conclusions and recommendations made by the participants. The publication also contains 13 individual presentations delivered by the participants. Each of the individual papers has been provided with an abstract and indexed separately

Report of the research co-ordination meeting on reference materials for microanalytical nuclear techniques

Energy Technology Data Exchange (ETDEWEB)

NONE

1994-07-01

Many microanalytical procedure require specific natural-matrix reference materials containing very low levels of trace elements and having a high degree of homogeneity. This proposed CRP will specifically address the question of quality control materials for these techniques. The participants of the meeting discussed the requirements for certified reference materials to by used in microanalysis with particular emphasis on the homogeneity issues. This publication contains summary of the discussions along with conclusions and recommendations made by the participants. The publication also contains 13 individual presentations delivered by the participants. Each of the individual papers has been provided with an abstract and indexed separately.

Certified reference materials for food packaging specific migration tests: development, validation and modelling

NARCIS (Netherlands)

Stoffers, N.H.

2005-01-01

Keywords:certified reference materials; diffusion; food contact materials; food packaging; laurolactam; migration modelling; nylon; specific migration This thesis compiles several research topics

Analysis of Reference Cigarette Smoke Yield Data From 21 Laboratories for 28 Selected Analytes as a Guide to Selection of New Coresta Recommended Methods

Directory of Open Access Journals (Sweden)

Purkis Steve

2014-07-01

Full Text Available Since 1999, the CORESTA Special Analytes Sub Group (SPA SG has been working on the development of CORESTA Recommended Methods (CRMs for the analysis of cigarette smoke components. All CRMs have been posted on the CORESTA website and several associated papers published. In this study, 21 laboratories shared data and in-house methodologies for 28 additional smoke components of regulatory interest to prioritise the development of further CRMs. Laboratories provided data, where available, from CORESTA monitor test pieces (CM6 and CM7 and Kentucky Reference Cigarettes (1R5F / 3R4F covering the period 2010-2012 obtained under both the ISO 3308 and Health Canada Intense regimes. Scant data were available on the CORESTA monitor test pieces and the Kentucky 1R5F reference. The greatest amount of data was obtained on the Kentucky 3R4F and this was used in the analyses described in this paper. SPA SG discussions provided invaluable insight into identifying causes and ways of reducing inter-laboratory variability which will be investigated in joint experiments before embarking on final collaborative studies using draft CRMs to obtain mean yields, repeatability and reproducibility values. Phenolic compounds (phenol, 3 cresol isomers, hydroquinone, catechol and resorcinol gave consistent results by liquid chromatography (LC separation and fluorescence detection after extracting collected “tar” on a Cambridge filter pad (CFP. Yields were similar to those obtained by a derivatisation method followed by gas chromatography - mass spectrometry (GC-MS analysis. Similar ratios of phenols were also obtained from each method. Of the 28 studied analytes, the between-laboratory variability was lowest for the phenols. Hydrogen cyanide was derivatised using various reagents and the colour development measured after continuous flow analysis (CFA by ultra-violet absorbance. Although, methodologies gave reasonably consistent results, investigations on the trapping system

Certification of mercury in acrylonitrile butadiene styrene by using isotope dilution mass spectrometry

International Nuclear Information System (INIS)

Hu Hai; Ma Liandi; Wei Chao; Zhou Tao; Wang Jun; Zhao Motian; Li Jinying

2008-01-01

Under the framework of a co-certification system for the development of Certified Reference Materials (CRMs) among China, Japan and Korea, the 1st co-certification campaign of mercury in acrylonitrile butadiene styrene (ABS) for Japanese CRMs was taken. In this campaign isotope dilution mass spectrometry (IDMS) was used. First, all abundances of Hg in spike 202 Hg, CRM and ABS were analyzed by MC-ICP-MS before the certification. Then the concentrations of 202 Hg and Hg in ABS were determined with IDMS by Q-ICP-MS. A new procedure to reduce memory effect was used. first, dilute with 5 μg/g Au solution for 1 min; then, 5 μg/g EDTA solution for 2 min. The results accord to each other very well and this implies that the co-certification system can run swimmingly. (authors)

Spiked environmental matrix for use as a reference material for gamma-ray spectrometry: Production and homogeneity test

International Nuclear Information System (INIS)

Sobiech-Matura, K.; Máté, B.; Altzitzoglou, T.

2016-01-01

The application of a spiking method for reference material production and its utilisation for a food matrix is presented. The raw rice powder was tested by means of γ-ray spectrometry and spiked with a "1"3"7Cs solution. The spiked material was mixed and tested for homogeneity. The future use of the rice powder reference material after the entire characterisation cycle will be for γ-ray spectrometry method validation. - Highlights: • Spiking blank substance with a traceable radioactive solution • Spiked reference material for γ-ray emitting radionuclides in food matrix • Results of the homogeneity tests are presented

Certified reference materials for analytical quality control in neutron activation analysis

International Nuclear Information System (INIS)

Wee Boon Siong; Abdul Khalik Wood; Mohd Suhaimi Hamzah; Shamsiah Abdul Rahman; Mohd Suhaimi Elias; Nazaratul Ashifa Abdul Salim

2007-01-01

Analytical quality control in neutron activation analysis (NAA) requires the use of certified reference materials (CRM) in order to produce reliable analytical results. It is essential to evaluate the performance of NAA method when analyzing various sample matrices. Therefore, the CRM selected for an analysis should be suitable for the type of samples. There are many aspects such as concentration range, matrix match, sample size and uncertainty, which need to be considered when selecting a suitable CRM. Eventually, results of analysis of CRM were plotted into control charts in order to evaluate the qualify of the data. This is to ensure that the results are within the 95 % confidence interval as stipulated in the certificate of CRM. Thus, this article aims to discuss the uses of certified reference materials for quality control purposes in NAA involving various sample matrices. (author)

Determination of uranium in tree bark samples by epithermal neutron activation analysis

International Nuclear Information System (INIS)

Lima, Nicole Pereira de; Saiki, Mitiko

2017-01-01

In this study uranium (U) concentrations were determined in certified reference materials (CRMs) and in tree bark samples collected in 'Cidade Universitaria Armando de Salles Oliveira' (CUASO) USP, Sao Paulo, SP, Brazil). The barks were collected from different species namely Poincianella pluviosa and Tipuana tipu. These bark samples were cleaned, dried, grated and milled for the analyses by epithermal neutron activation analysis method (ENAA). This method consists on irradiating samples and U standard in IEAR1 nuclear reactor with thermal neutron flux of 1:9 x 10 12 n cm -2 s -1 during 40 to 60 seconds depending on the samples matrices. The samples and standard were measured by gamma ray spectroscopy. U was identified by the peak of 74.66 keV of 239 U with half life of 23.47 minutes. Concentration of U was calculated by comparative method. For analytical quality control of U results, certified reference materials were analysed. Results obtained for CRMs presented good precision and accuracy, with |Z score| <= 0.39. Uranium concentrations in tree barks varied from 83.1 to 627.6 ng g - 1 and the relative standard deviations of these results ranged from 1.8 to 10%. (author)

Determination of uranium in tree bark samples by epithermal neutron activation analysis

Energy Technology Data Exchange (ETDEWEB)

Lima, Nicole Pereira de; Saiki, Mitiko, E-mail: mitiko@ipen.com [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

2017-11-01

In this study uranium (U) concentrations were determined in certified reference materials (CRMs) and in tree bark samples collected in 'Cidade Universitaria Armando de Salles Oliveira' (CUASO) USP, Sao Paulo, SP, Brazil). The barks were collected from different species namely Poincianella pluviosa and Tipuana tipu. These bark samples were cleaned, dried, grated and milled for the analyses by epithermal neutron activation analysis method (ENAA). This method consists on irradiating samples and U standard in IEAR1 nuclear reactor with thermal neutron flux of 1:9 x 10{sup 12} n cm{sup -2} s{sup -1} during 40 to 60 seconds depending on the samples matrices. The samples and standard were measured by gamma ray spectroscopy. U was identified by the peak of 74.66 keV of {sup 239}U with half life of 23.47 minutes. Concentration of U was calculated by comparative method. For analytical quality control of U results, certified reference materials were analysed. Results obtained for CRMs presented good precision and accuracy, with |Z score| <= 0.39. Uranium concentrations in tree barks varied from 83.1 to 627.6 ng g{sup -} {sup 1} and the relative standard deviations of these results ranged from 1.8 to 10%. (author)

Need for organic reference materials in marine science

Energy Technology Data Exchange (ETDEWEB)

Wells, D.E.

1988-12-01

The reference materials (RMs) available for organic trace analysis (OTA) and the development programmes of the RM producers are reviewed. The need for a wider range of determinants, matrices and classes of RMs, particularly the more widespread use of laboratory RMs (LRMs) is discussed. Additional certified RMs should include phenolic surfactant degradation products, chlorophenolics from the wood and paper industries, and organobromines from fire retardants. RMs as molecular markers of geogenic, pyrogenic and biogenic sources; chlorophylls and xanthophylls as a measure of marine productivity and natural shellfish toxins are proposed.

Certified reference materials for the determination of mineral oil hydrocarbons in water, soil and waste

Energy Technology Data Exchange (ETDEWEB)

Koch, M.; Liebich, A.; Win, T.; Nehls, I.

2005-07-01

The international research project HYCREF, funded by the European Commission in the 5{sup th} Framework programme, aimed to develop methods to prepare homogeneous and stable water-, soil- and waste reference materials contaminated with mineral oil hydrocarbons and to test certify the mineral oil content by gas chromatographic methods. As mineral oil products are important sources for environmental contaminations a high need exists for certified reference materials for their determination using the new gas chromatographic methods (soil: ISO/FDIS 16703, waste: ENpr 14039, water: ISO 9377-2). The experimental conditions and results for preparation and characterisation of a total of nine reference materials (3 water, 3 soil- and 3 waste materials) are described and discussed. Target values for the reference materials were defined at the beginning of the project in order to have clear quality criteria, which could be compared with the achieved results at the end of the project. These target specifications were related to the maximum uncertainty from test certification exercises (<5% for soil/waste and <10% for water), the maximum inhomogeneity between bottles (<3%) and minimum requirements for stability (>5 years for soil/waste and >2 years for water). The feasibility studies showed that solid materials (soil, waste) could be prepared sufficiently homogeneous and stable. The test certified values of the 6 solid materials comprise a wide range of mineral oil content from about 200-9000 mg/kg with expanded uncertainties between 5.7-13.1% using a coverage factor k (k=2). The development of new water reference materials - the so-called ''spiking pills'' for an offshore- and a land-based discharge water represents one of the most innovative aspects of the project. The spiking pill technology facilitates the application and storage and improves the material stability compared with aqueous materials. Additional to the preparation and test certification of

Chemical analysis of high purity graphite

International Nuclear Information System (INIS)

1993-03-01

The Sub-Committee on Chemical Analysis of Graphite was organized in April 1989, under the Committee on Chemical Analysis of Nuclear Fuels and Reactor Materials, JAERI. The Sub-Committee carried out collaborative analyses among eleven participating laboratories for the certification of the Certified Reference Materials (CRMs), JAERI-G5 and G6, after developing and evaluating analytical methods during the period of September 1989 to March 1992. The certified values were given for ash, boron and silicon in the CRM based on the collaborative analysis. The values for ten elements (Al, Ca, Cr, Fe, Mg, Mo, Ni, Sr, Ti, V) were not certified, but given for information. Preparation, homogeneity testing and chemical analyses for certification of reference materials were described in this paper. (author) 52 refs

Development of Microanaytical Reference Materials for In-situ Anaysis at the U.S. Geological Survey

Science.gov (United States)

Wilson, S.

2006-05-01

With the increased use of microanalysis in geochemical investigations comes the need for a reliable and diversified supply of reference materials homogenous at the micrometer scale to assist analysts in element quantification. To meet these requirements, the U.S. Geological Survey (USGS) has undertaken a program to develop a series of reference materials which cover a range of sample types currently being investigated in our microanalytical laboratories. Initial efforts have focused on the development of natural basalt glasses (BCR- 2G, BHVO-2G, BIR-1G, TB-1G, NKT-1G) from a variety of geologic settings. In addition to these natural basalt materials a series of synthetic basalt glasses GSA-1G, GSC-1G, GSD-1G, GSE-1G have also been developed with 65 trace elements at 0, 3, 30, and 300, ppm respectively. The homogeneity of these materials and their use in international microanalytical proficiency studies will be presented. Application of this technology to the development of glass reference materials as part of a USGS/NASA collaborative studies on the development of Lunar Soil Simulant material will also be discussed.

The determination, by instrumental neutron-activation analysis, of some elements in the NIMROC standard reference materials

International Nuclear Information System (INIS)

Eddy, B.T.; Pearton, D.C.G.; Bibby, D.M.

1975-01-01

Instrumental neutron-activation analysis was used for the determination of sixteen trace and minor elements in the six NIMROC reference materials. Six reference rock materials prepared by the U.S. Geological Survey were also analysed, and the results were compared with the recommended, average, or magnitude values given for these rocks by Flanagan. The agreement between the two sets of results was found to be generally good, indicating that INAA is an acceptable technique for the determination of most of these elements. The values found for the NIMROC samples represent a significant contribution to the evaluation of the trace elements in these reference materials [af

Accurate determination of trace amounts of lanthanum, yttrium and all stable lanthanides in biological materials by Ion Chromatography

International Nuclear Information System (INIS)

Dybczynski, R.S.; Kulisa, K.; Danko, B.; Samczynski, Z.

2007-01-01

The analytical procedure for the isolation and preconcentration of La, Y and the lanthanides from biological materials and their determination by ion chromatography (IC) with the use of Dionex Ion Pac CS3 + CG3 column (sulfonic acid type), α-hydroxyisobutyric acid (α-HIBA) as an eluent, and PAR or Arsenazo III as color forming reagents, was elaborated. The scheme originally devised for NAA, involving microwave assisted digestion and multi step separation employing ion exchange and extraction chromatography columns was used to selectively recover REE fraction (without scandium) with 100% yield. The REE fraction was analyzed by IC at 25 and 70 o C. The run at 70 o C enabled resolution of Y and Dy peaks and as a result made possible quantitative determination of La, Y, and all lanthanides. Investigation on the mechanism of band spreading revealed that longitudinal diffusion in the stationary phase considerably contributed to the total plate height. Surprisingly, the plate height (H) calculated from Y peak was distinctly lower than H values of the adjacent lanthanides. The method was validated by analyzing several certified reference materials (CRMs). (authors)

Committee on Diabetes Mellitus Indices of the Japan Society of Clinical Chemistry-recommended reference measurement procedure and reference materials for glycated albumin determination.

Science.gov (United States)

Takei, Izumi; Hoshino, Tadao; Tominaga, Makoto; Ishibashi, Midori; Kuwa, Katsuhiko; Umemoto, Masao; Tani, Wataru; Okahashi, Mikiko; Yasukawa, Keiko; Kohzuma, Takuji; Sato, Asako

2016-01-01

Glycated albumin is an intermediate glycaemic control marker for which there are several measurement procedures with entirely different reference intervals. We have developed a reference measurement procedure for the purpose of standardizing glycated albumin measurements. The isotope dilution liquid chromatography/tandem mass spectrometry method was developed as a reference measurement procedure for glycated albumin. The stable isotopes of lysine and fructosyl-lysine, which serve as an internal standard, were added to albumin isolated from serum, followed by hydrogenation. After hydrolysis of albumin with hot hydrochloric acid, the liberated lysine and fructosyl-lysine were measured by liquid chromatography/tandem mass spectrometry, and their concentrations were determined from each isotope ratio. The reference materials (JCCRM611) for determining of glycated albumin were prepared from pooled patient blood samples. The isotope dilution-tandem mass spectrometry calibration curve of fructosyl-lysine and lysine showed good linearity (r = 0.999). The inter-assay and intra-assay coefficient of variation values of glycated albumin measurement were 1.2 and 1.4%, respectively. The glycated albumin values of serum in patients with diabetes assessed through the use of this method showed a good relationship with routine measurement procedures (r = 0.997). The relationship of glycated albumin values of the reference material (JCCRM611) between these two methods was the same as the relationship with the patient serum samples. The Committee on Diabetes Mellitus Indices of the Japan Society of Clinical Chemistry recommends the isotope dilution liquid chromatography/tandem mass spectrometry method as a reference measurement procedure, and JCCRM611 as a certified reference material for glycated albumin measurement. In addition, we recommend the traceability system for glycated albumin measurement. © The Author(s) 2015.

On the interpretation of micro-PIXE measurements on a prototype microstructured reference material

International Nuclear Information System (INIS)

Waetjen, Uwe; Barsony, Istvan; Grime, Geoff W.; Rajta, Istvan

1999-01-01

In order to determine the beam spot size and scanning properties of ion microbeam systems, a novel reference material has been developed, consisting of permalloy (81% Ni, 19% Fe) strip patterns on silicon substrate. Due to the choice of substrate and pattern materials, these samples exhibit a high elemental contrast suitable for analysis with X-ray detection and ion scattering techniques. The microlithographic production scheme is briefly described. A prototype chip of this material was investigated with PIXE and RBS analysis in a scanning nuclear microprobe. It proved to be extremely useful in the routine to focus the ion microbeam and to determine its spot size. Due to the microscopic structure of these samples, a geometric dependence of matrix effects in the production of Si X-rays from the substrate material could be shown. Even dead-time effects in the counting electronics, showing up as an apparent thickness gradient, could be observed. Besides its primary role in microbeam diagnostics, this reference material can serve an educational role in developing the analyst's ability to correctly identify and interpret such artefacts

Measurements Matter in Nuclear Safeguards & Security

International Nuclear Information System (INIS)

Aregbe, Y.; Jakopic, R.; Richter, S.; Schillebeeckx, P.; Hult, M.

2015-01-01

The deliverable of any laboratory is a measurement result with stated uncertainty and traceability (ISO/IEC 17025: 2005). Measurement results, particularly in safeguards, have to be accurate, comparable and traceable to a stated reference, preferably to the SI. Results provided by operator-, safeguards- or network laboratories have to be in compliance with specific quality goals for nuclear material and environmental sample analysis. Metrological quality control tools are prerequisites to build up confidence in measurement results that have to be translated into meaningful safeguards conclusions or to demonstrate conformity of findings with declared processes. The European Commission—Joint Research Centre (EC–JRC) has dedicated facilities, laboratories and projects to provide certified nuclear reference materials (CRM), to develop reference methods and to organize inter-laboratory comparisons (ILC) in compliance with ISO Guide 34, ISO17025 and ISO17043, including respective training. Recent examples are: – cooperation with the JAEA to investigate on the application of Neutron Resonance Densitometry (NRD) to quantify the amount of special nuclear material in particlelike debris of melted fuel as formed in the nuclear accident in Fukushima – training in metrology and gamma-ray spectrometry for EURATOM safeguards inspectors – development of uranium reference particle standards under a new EC support task to the IAEA. Currently, the JRC puts major efforts in producing CRMs and conformity assessment tools for “age-dating” of uranium and plutonium samples. They are needed for method validation in determining the date of the last chemical separation of uranium or plutonium from their daughter nuclides. These type of CRMs are not only needed in nuclear safeguards and forensics, but could support in the future a possible new type of “verification mechanism” as part of the Fissile Material Cut-off Treaty (FMCT), since measurements and measurement standards

A study of production of radioactive environmental reference materials used for proficiency testing program in Taiwan

International Nuclear Information System (INIS)

Peng, En-Chi; Wang, Jeng-Jong

2013-01-01

To realise radioactive environmental reference materials in Taiwan, seven environmental materials of soil, water, vegetation, meat, airborne particles (filter paper), milk and mushroom samples that are frequently encountered were used to establish the preparation of the reference materials. These seven environmental materials were collected, checked for freedom from radioactivity and prepared according to their properties. The preparation was carried out by using activity about 10–100 times that of the minimum detectable activity (MDA) in routine measurements in the radioactive standard used to spike the inactive material and this standard is traceable to national ionising radioactivity standards (TAF, 2004). To demonstrate sample traceability to the added standard, each sample was carefully measured and its uncertainty evaluated. Based on the recommendations of ISO Guide 35 for evaluation of reference materials and with the above assessment and verification procedures, the uncertainties (k=1) of the spike activity used in making reference materials were: 60 Co≤4.6%, 134 Cs≤4.7%, 137 Cs≤5.0%, total β≤0.6% and 3 H≤1.3%. - Highlights: • Seven kinds environmental materials were used to establish the production of the RMs. • Spiking the traceable standard radioactive source to the blank substance. • Each sample was carefully evaluated for its uncertainty. • The performance of the RMs was estimated with the Proficiency Testing program report. • The ability of the environment RMs in the configuration is quite good

Certification of a uranium dioxide reference material for chemical analyses

International Nuclear Information System (INIS)

Le Duigou, Y.

1984-01-01

This report, issued by the Central Bureau for Nuclear Measurements (CBNM), describes the characterization of a uranium dioxide reference material with accurately determined uranium mass fraction for chemical analyses. The preparation, conditioning, homogeneity tests and the analyses performed on this material are described in Annex 1. The evaluation of the individual impurity results, total of impurities and uranium mass fraction are given in Annex 2. Information on a direct determination of uranium by titration is given in Annex 3. The uranium mass fraction (881.34+-0.13) g.kg -1 calculated in Annex 2 is given on the certificate

Determination of platinum-group elements in the geological standard reference materials by isotope dilution-ICPMS

Energy Technology Data Exchange (ETDEWEB)

Mingyue, Hu; Hongliao, He [National Research Center for Geoanalysis, Beijing (China)

2005-10-15

Platinum group elements (PGEs) includes platinum, palladium, iridium, osmium, rhodium and ruthenium. It has very high economic and scientific value in the field of geoscience and environmental science. But the analysis data referred by the different lab are very disperse because of the difficulty of the determination of PGEs. It makes very difficult to fix the value of the PGEs in the standard reference materials. In the article, the values of the PGEs in the standard reference materials of ocean sediment are determined by isotope dilution technique and dependable values of these elements are provided. (authors)

Determination of platinum-group elements in the geological standard reference materials by isotope dilution-ICPMS

International Nuclear Information System (INIS)

Hu Mingyue; He Hongliao

2005-01-01

Platinum group elements (PGEs) includes platinum, palladium, iridium, osmium, rhodium and ruthenium. It has very high economic and scientific value in the field of geoscience and environmental science. But the analysis data referred by the different lab are very disperse because of the difficulty of the determination of PGEs. It makes very difficult to fix the value of the PGEs in the standard reference materials. In the article, the values of the PGEs in the standard reference materials of ocean sediment are determined by isotope dilution technique and dependable values of these elements are provided. (authors)

The NISTmAb Reference Material 8671 lifecycle management and quality plan.

Science.gov (United States)

Schiel, John E; Turner, Abigail

2018-03-01

Comprehensive analysis of monoclonal antibody therapeutics involves an ever expanding cadre of technologies. Lifecycle-appropriate application of current and emerging techniques requires rigorous testing followed by discussion between industry and regulators in a pre-competitive space, an effort that may be facilitated by a widely available test metric. Biopharmaceutical quality materials, however, are often difficult to access and/or are protected by intellectual property rights. The NISTmAb, humanized IgG1κ Reference Material 8671 (RM 8671), has been established with the intent of filling that void. The NISTmAb embodies the quality and characteristics of a typical biopharmaceutical product, is widely available to the biopharmaceutical community, and is an open innovation tool for development and dissemination of results. The NISTmAb lifecyle management plan described herein provides a hierarchical strategy for maintenance of quality over time through rigorous method qualification detailed in additional submissions in the current publication series. The NISTmAb RM 8671 is a representative monoclonal antibody material and provides a means to continually evaluate current best practices, promote innovative approaches, and inform regulatory paradigms as technology advances. Graphical abstract The NISTmAb Reference Material (RM) 8671 is intended to be an industry standard monoclonal antibody for pre-competitive harmonization of best practices and designing next generation characterization technologies for identity, quality, and stability testing.

A comparison of chemical reference materials for solution calorimeters.

Science.gov (United States)

Ramos, Rita; Gaisford, Simon; Buckton, Graham; Royall, Paul G; Yff, Barbara T S; O'Neill, Michael A A

2005-08-11

Solution calorimeters are based on semi-adiabatic or isothermal heat-conduction principles and differ in the way they record data. They also have different measuring sensitivities and require different quantities of solute and solvent. As such, the choice of chemical test substance is not straightforward. Usually the dilution of KCl is recommended; it is possible to purchase a reference sample of KCl that has a certified enthalpy of solution and this standard material is usually used to test semi-adiabatic instruments. Here, we review the suitability of a range of chemical test substances (KCl, sucrose and Tris) for an isothermal heat-conduction solution calorimeter. It was found that KCl was not the best test material because its relatively high enthalpy of solution (DeltasolH) necessitated the use of small samples (2 mg), resulting in a relatively large standard deviation (sigman-1) in the values recorded (DeltasolH=17.14+/-0.49 kJ mol-1); furthermore, KCl data must be corrected to account for the effect of dilution, although the correction was found to be small (0.07 kJ mol-1) under the experimental conditions employed here. Sucrose appears to be a much more robust test material for isothermal heat-conduction instruments because its lower enthalpy of solution allows the use of much larger samples (20 mg), which minimises experimental errors. The DeltasolH value returned (6.14+/-0.08 kJ mol-1) is in excellent agreement with the literature. It is also cheap, readily available and requires minimal preparation although its widespread use would require the preparation of a certified reference sample.

Halogens determination in vegetable NBS standard reference materials

International Nuclear Information System (INIS)

Stella, R.; Genova, N.; Di Casa, M.

1977-01-01

Levels of all four halogens in Orchard Leaves, Pine Needles and Tomato Leaves NBS reference standards were determined. For fluorine a spiking isotope dilution method was used followed by HF absorption on glass beads. Instrumental nuclear activation analysis was adopted for chlorine and bromine determination. Radiochemical separation by a distillation procedure was necessary for iodine nuclear activation analysis after irradiation. Activation parameters of Cl, Br and I are reported. Results of five determinations for each halogen in Orchard Leaves, Pine Needles and Tomato Leaves NBS Standard Materials and Standard deviations of the mean are reported. (T.I.)

Development of new reference materials for the determination of cadmium, chromium, mercury and lead in polycarbonate

International Nuclear Information System (INIS)

Lee, Kil Jae; Lee, Yeo Jin; Choi, Young Rak; Kim, Jeong Sook; Kim, Youn Sung; Heo, Soo Bong

2013-01-01

Highlights: ► RMs for the determination of Cd, Cr, Hg and Pb in polycarbonate were developed. ► Double ID-ICP-MS technique was used for characterization of candidate RMs. ► The certified values for the elements ranged from 51.7 to 1133 mg kg −1 . ► The relative expanded uncertainties were shown to be less than 5.4%. ► New RMs were found to be suitable for the RoHS compliant tests. - Abstract: Reference materials for quantitative determination of Cd, Cr, Hg and Pb in polycarbonate were developed. Reference materials with two concentration level of elements were prepared by adding appropriate amounts of chemicals to a blank polycarbonate base material. It was shown that ten bottles with triplicate analysis are enough to demonstrate the homogeneity of these candidate reference materials. The statistical results also showed no significant trends in both short-term stability test for four weeks and long-term stability test for twelve months. The certification of the four elements was carried out by isotope-dilution-inductively coupled plasma mass spectrometry (ID-ICP-MS) with microwave-assisted digestion. Certification of candidate reference materials in a single laboratory was confirmed with interlaboratory comparison participated by a certain number of well-recognized testing laboratories in Korea. The certified values and expanded uncertainties (k = 2) for the candidate reference material with low level and the one with high level were (51.7 ± 2.1) mg kg −1 Cd, (103.8 ± 2.9) mg kg −1 Cd, (98.8 ± 4.5) mg kg −1 Cr, (1004 ± 49.8) mg kg −1 Cr, (107.4 ± 4.6) mg kg −1 Hg, (1133 ± 50.7) mg kg −1 Hg, (94.8 ± 3.7) mg kg −1 Pb and (988.4 ± 53.6) mg kg −1 Pb, respectively. The reference materials developed in this study demonstrated their suitability for the quality assurance in Cd, Cr, Hg and Pb analysis for the implementation of RoHS Directive.

NKS-Norcmass reference material for analysis of Pu-isotopes and 237Np by mass spectrometry

International Nuclear Information System (INIS)

Ross, P.; Nygren, U.; Appelblad, P.; Skipperud, L.; Sjoegren, A.

2006-04-01

The aim of the reference material in the Norcmass-project was to produce a low-level ( 239 Pu) sample of sufficient amount to allow individual laboratories to perform several tests without risk of using up the material. Although there are several reference materials available (eg IAEA) few have 239 Pu/ 240 Pu data and almost none have 237 Np/ 239 Pu-data. Those who have (eg IAEA-384) have very high concentrations and are not useful for testing analytical methods designed for low-level measurements where a large sample mass may be required. The reference material consist of the top 10cm of 2mm sieved soil pooled together from 12 different Danish locations collected during 2003. The Soil was blended and sieved through 0.6 and finally through a 0.4 mm sieve. A total amount of 17 kg soil was produced. Several aliquots of the material was subject to analysis by alpha spectrometry and ICP-MS. The material contain 239 + 240 Pu at a concentration of 0.24 ± 0.01 mBq/g and a 240 Pu/ 239 Pu atom ratio of 0.19 ± 0.006. The ratio 237 Np/ 239 Pu was determined to 0.32 ± 0.01. (au)

Instrumental neutron activation analysis of proposed marine sediment reference material (IAEA-158)

International Nuclear Information System (INIS)

Siddique, N.; Waheed, S.

2009-01-01

IAEA-158, sediment prepared by the International Atomic Energy Agency -Marine Environmental Laboratory (IAEA-MEL), Monaco was received under the IAEA Analytical Quality Control Services (AQCS) Intercomparison Programme. Instrumental Neutron Activation Analysis (INAA) was used to determine AI, As, Br, Ce, Co, Cr, Cs, Eu, Fe, Hf, K, La, Lu, Mn, Na, Nd, Rb, Sb, Sc, Se, Sm, Ta, Tb, Th, V, Vb and Zn in this proposed reference material (RM). Four different irradiation protocols were adopted using a miniature neutron source reactor (MNSR) by varying the irradiation, cooling and counting times. IAEA-405 (Estuarine Sediment) and IAEA-SLI (Lake Sediment) were used as compatible matrix reference materials for quality assurance (QA) purposes. Good agreement between our data and lAEA certified values was obtained providing confidence in the reported data. (author)

Instrumental neutron and photon activation analyses of selected geochemical reference materials

Czech Academy of Sciences Publication Activity Database

Mizera, Jiří; Řanda, Z.

2010-01-01

Roč. 284, č. 1 (2010), s. 157-163 ISSN 0236-5731 Institutional research plan: CEZ:AV0Z30460519 Keywords : neutron activation analysis * photon activation analysis * geochemical reference materials Subject RIV: BG - Nuclear, Atomic and Molecular Physics, Colliders OBOR OECD: Analytical chemistry Impact factor: 0.777, year: 2010

Establishing the traceability of a uranyl nitrate solution to a standard reference material

International Nuclear Information System (INIS)

Jackson, C.H.; Clark, J.P.

1978-01-01

A uranyl nitrate solution for use as a Working Calibration and Test Material (WCTM) was characterized, using a statistically designed procedure to document traceability to National Bureau of Standards Reference Material (SPM-960). A Reference Calibration and Test Material (PCTM) was prepared from SRM-960 uranium metal to approximate the acid and uranium concentration of the WCTM. This solution was used in the characterization procedure. Details of preparing, handling, and packaging these solutions are covered. Two outside laboratories, each having measurement expertise using a different analytical method, were selected to measure both solutions according to the procedure for characterizing the WCTM. Two different methods were also used for the in-house characterization work. All analytical results were tested for statistical agreement before the WCTM concentration and limit of error values were calculated. A concentration value was determined with a relative limit of error (RLE) of approximately 0.03% which was better than the target RLE of 0.08%. The use of this working material eliminates the expense of using SRMs to fulfill traceability requirements for uranium measurements on this type material. Several years' supply of uranyl nitrate solution with NBS traceability was produced. The cost of this material was less than 10% of an equal quantity of SRM-960 uranium metal

Catalog of NBS standard reference materials, 1975--76 edition. Special pub

International Nuclear Information System (INIS)

Seward, R.W.

1975-06-01

This Catalog lists and describes the Standard Reference Materials (SRM's), Research Materials (RM's), and General Materials (GM's) currently distributed by the National Bureau of Standards, as well as many of the materials currently in preparation. SRM's are used to calibrate measurement systems and to provide a central basis for uniformity and accuracy of measurement. The unit and quantity, the type, and the certified characterization are listed for each SRM, as well as directions for ordering. The RM's are not certified, but are issued to meet the needs of scientists engaged in materials research. RM's are issued with a 'Report of Investigation', the sole authority of which is the author of the report. The GM's are standardized by some agency other than NBS. NBS acts only as a distribution point and does not participate in the standardization of these materials. Announcements of new and renewal SRM's, RM's and GM's are made in the semi-annual supplements of this Catalog, SRM Price List, and in scientific and trade journals

Aluminium-gold reference material for the k0-standardisation of neutron activation analysis

International Nuclear Information System (INIS)

Ingelbrecht, C.; Peetermans, F.; Corte, F. de; Wispelaere, A. de; Vandecasteele, C.; Courtijn, E.; Hondt, P. d'

1991-01-01

Gold is an excellent comparator material for the k 0 -standardisation of neutron activation analysis because of its convenient and well defined nuclear properties. The most suitable form for a reference material is a dilute aluminium-gold alloy, for which the self-shielding effect for neutrons is small. Castings of composition Al-0.1 wt.% Au were prepared by crucible-less levitation melting, which gives close control of ingot composition with minimal contamination of the melt. The alloy composition was checked using induction-coupled plasma source emission spectrometry. The homogeneity of the alloy was measured by neutron activation analysis and a relative standard deviation of the gold content of 0.30% was found (10 mg samples). Metallography revealed a homogeneous distribution of AuAl 2 particles. The alloy was certified as Reference Materials CBNM-530, with certified gold mass fraction 0.100±0.002 wt.%. (orig.)

Short-term stability test for thorium soil candidate a reference material

Energy Technology Data Exchange (ETDEWEB)

Clain, Almir F.; Fonseca, Adelaide M.G.; Dantas, Vanessa V.D.B.; Braganca, Maura J.C.; Souza, Poliana S., E-mail: almir@ird.gov.br, E-mail: adelaide@ird.gov.br, E-mail: vanessa@ird.gov.br, E-mail: maura@ird.gov.br, E-mail: poliana@bolsista.ird.gov.br [Instituto de Radioprotecao e Dosimetria (IRD/CNEN-RJ), Rio de Janeiro, RJ (Brazil)

2015-07-01

This work describes a methodology to determine the soil short-term stability after the steps of production in laboratory. The short-term stability of the soil is an essential property to be determined in order to producing a reference material. The soil is a candidate of reference material for chemical analysis of thorium with metrological traceability to be used in environmental analysis, equipment calibration, validation methods, and quality control. A material is considered stable in a certain temperature if the property of interest does not change with time, considering the analytical random fluctuations. Due to this, the angular coefficient from the graphic of Th concentration versus elapsed time must be near to zero. The analytical determinations of thorium concentration were performed by Instrumental Neutron activation Analysis. The slopes and their uncertainties were obtained from the regression lines at temperatures of 20 deg C and 60 deg C, with control temperature of -20 deg C. From the obtained data a t-test was applied. In both temperatures the calculated t-value was lower than the critical value, so we can conclude with 95% confidence level that no significant changes happened during the period studied concerning thorium concentration in soil at temperatures of 20 deg C and 60 deg C, showing stability at these temperatures. (author)

Short-term stability test for thorium soil candidate a reference material

International Nuclear Information System (INIS)

Clain, Almir F.; Fonseca, Adelaide M.G.; Dantas, Vanessa V.D.B.; Braganca, Maura J.C.; Souza, Poliana S.

2015-01-01

This work describes a methodology to determine the soil short-term stability after the steps of production in laboratory. The short-term stability of the soil is an essential property to be determined in order to producing a reference material. The soil is a candidate of reference material for chemical analysis of thorium with metrological traceability to be used in environmental analysis, equipment calibration, validation methods, and quality control. A material is considered stable in a certain temperature if the property of interest does not change with time, considering the analytical random fluctuations. Due to this, the angular coefficient from the graphic of Th concentration versus elapsed time must be near to zero. The analytical determinations of thorium concentration were performed by Instrumental Neutron activation Analysis. The slopes and their uncertainties were obtained from the regression lines at temperatures of 20 deg C and 60 deg C, with control temperature of -20 deg C. From the obtained data a t-test was applied. In both temperatures the calculated t-value was lower than the critical value, so we can conclude with 95% confidence level that no significant changes happened during the period studied concerning thorium concentration in soil at temperatures of 20 deg C and 60 deg C, showing stability at these temperatures. (author)

River bottom sediment from the Vistula as matrix of candidate for a new reference material.

Science.gov (United States)

Kiełbasa, Anna; Buszewski, Bogusław

2017-08-01

Bottom sediments are very important in aquatic ecosystems. The sediments accumulate heavy metals and compounds belonging to the group of persistent organic pollutants. The accelerated solvent extraction (ASE) was used for extraction of 16 compounds from PAH group from bottom sediment of Vistula. For the matrix of candidate of a new reference material, moisture content, particle size, loss on ignition, pH, and total organic carbon were determined. A gas chromatograph with a selective mass detector (GC/MS) was used for the final analysis. The obtained recoveries were from 86% (SD=6.9) for anthracene to 119% (SD=5.4) for dibenzo(ah)anthracene. For the candidate for a new reference material, homogeneity and analytes content were determined using a validated method. The results are a very important part of the development and certification of a new reference materials. Copyright © 2017 Elsevier Inc. All rights reserved.

An attempt to prepare and characterize a soil reference material for Cr(VI) and Cr(III)

International Nuclear Information System (INIS)

Solano, G.; Katz, S.A.; Holzbecher, J.; Chatt, A.

1994-01-01

Reference materials for the speciation and quantification of chromium in contaminated soils were prepared by impregnating diatomaceous earth with BaCrO 4 and Cr 2 O 3 . The chromium concentrations of these materials were confirmed to be 200 mg/kg both by atomic absorption spectrometry and by instrumental neutron activation analysis, but monthly assays over two calendar quarters of the reference material impregnated with BaCrO 4 revealed the hexavalent chromium was not stable in this matrix. (author) 6 refs,; 2 tabs

A study on homogeneity of the IAEA candidate reference materials for microanalysis and analytical support in the certification of these materials

International Nuclear Information System (INIS)

Dybczynski, R.; Danko, B.; Polkowska-Motrenko, H.

2002-01-01

In this paper a study on homogeneity of new IAEA candidate reference materials: IAEA 338 Lichen and IAEA 413 Algae in small (ca.10 mg) samples as well as some data contributing to certification of these materials are presented. (author)

Development, Optimization, and Evaluation of a Duplex Droplet Digital PCR Assay To Quantify the T-nos/hmg Copy Number Ratio in Genetically Modified Maize.

Science.gov (United States)

Félix-Urquídez, Dalmira; Pérez-Urquiza, Melina; Valdez Torres, José-Benigno; León-Félix, Josefina; García-Estrada, Raymundo; Acatzi-Silva, Abraham

2016-01-05

Certified reference materials (CRMs) are required to guarantee the reliability of analytical measurements. The CRMs available in the field of genetically modified organisms (GMOs) are characterized using real-time polymerase chain reaction (qPCR). This technology has limited application, because of its dependence on a calibrant. The objective of this study was to obtain a method with higher metrological quality, to characterize the CRMs for their contents of T-nos/hmg copy number ratio in maize. A duplex droplet digital PCR (ddPCR) assay was developed and optimized by a central composite design. The developed method achieved an absolute limit of detection (LOD) of 11 cP T-nos, a relative LOD of 0.034%, a limit of quantification (LOQ) of 23 cP (relative LOQ of 0.08%), and a dynamic range of 0.08%-100% T-nos/hmg ratio. The specificity and applicability of the assay were established for the analysis of low T-nos concentrations (0.9%) in several corn varieties. The convenience of DNA digestion to reduce measurement bias in the case of multiple-copy binding was confirmed through an enzymatic restriction assay. Given its overall performance, this method can be used to characterize CRM candidates for their contents of T-nos/hmg ratio.

Development, Optimization, and Evaluation of a Duplex Droplet Digital PCR Assay To Quantify the T-nos/hmg Copy Number Ratio in Genetically Modified Maize

Science.gov (United States)

2015-01-01

Certified reference materials (CRMs) are required to guarantee the reliability of analytical measurements. The CRMs available in the field of genetically modified organisms (GMOs) are characterized using real-time polymerase chain reaction (qPCR). This technology has limited application, because of its dependence on a calibrant. The objective of this study was to obtain a method with higher metrological quality, to characterize the CRMs for their contents of T-nos/hmg copy number ratio in maize. A duplex droplet digital PCR (ddPCR) assay was developed and optimized by a central composite design. The developed method achieved an absolute limit of detection (LOD) of 11 cP T-nos, a relative LOD of 0.034%, a limit of quantification (LOQ) of 23 cP (relative LOQ of 0.08%), and a dynamic range of 0.08%–100% T-nos/hmg ratio. The specificity and applicability of the assay were established for the analysis of low T-nos concentrations (0.9%) in several corn varieties. The convenience of DNA digestion to reduce measurement bias in the case of multiple-copy binding was confirmed through an enzymatic restriction assay. Given its overall performance, this method can be used to characterize CRM candidates for their contents of T-nos/hmg ratio. PMID:26605751

Characterization of the NIST shellfish Standard Reference Material 4358

International Nuclear Information System (INIS)

Nour, S.; Inn, K.G.W.; Filliben, J.; Gaast van der, H.; Men, L.C.; Calmet, D.; Altzitzoglou, T.; Povinec, P.; Takata, Y.; Wisdom, M.

2013-01-01

A new shellfish Standard Reference Material 4358 was developed by the National Institute of Standards and Technology through an international interlaboratory comparison that involved twelve laboratories-participants from nine countries. The results from the participants were statistically evaluated, and the most robust certified values were based on the median of laboratories’ reported means and the uncertainties derived using the bootstrap method. Massic activity certified values were established for fourteen radionuclides, five activity ratios, and informational massic activity values for eight more radionuclides and two activity ratios. (author)

Preliminary homogeneity study of in-house reference material using neutron activation analysis and X-ray fluorescence

International Nuclear Information System (INIS)

Gras, N.; Munoz, L.; Cassorla, V.; Castillo, P.

1993-01-01

Although many biological reference materials for quality control of trace element analysis are commercially available, there is still a need for additional local materials for special matrices. In the Latin American region a preliminary study has been commenced involving analytical strategies for the characterization of in-house reference material. A biological sample, prepared in Brazil, constitutes the first regional attempt to prepare reference material. It was analyzed by neutron activation analysis (NAA) and X-ray fluorescence (XRF) to verify its homogeneity. The determination of the trace elements and certain major elements was carried out by instrumental NAA. Trace elements such as Cd, Mn, Mo and Cu were determined using NAA with radiochemical separations to improve the sensitivity and precision. XRF was applied only to major constituents and some trace elements with concentration of more than 10 μg/g. From a total of 18 elements analyzed, only Fe, Cr and Sc were not homogeneously distributed. (orig.)

Instrumental neutron and photon activation analyses of selected geochemical reference materials

Czech Academy of Sciences Publication Activity Database

Mizera, Jiří; Řanda, Zdeněk

2010-01-01

Roč. 284, č. 1 (2010), s. 157-163 ISSN 0236-5731 R&D Projects: GA AV ČR IAA300130706 Institutional research plan: CEZ:AV0Z10480505 Keywords : neutron activation analysis * photon activation analysis * geochemical reference materials Subject RIV: BG - Nuclear, Atomic and Molecular Physics, Colliders Impact factor: 0.777, year: 2010

Determination of rare earth elements in the biological reference materials Pine Needles and Spruce Needles by neutron activation analysis

International Nuclear Information System (INIS)

Machado, C.N.; Maria, S.P.; Saiki, M.; Figueiredo, A.M.G.

1998-01-01

Instrumental neutron activation analysis was applied to determine La, Ce, Nd, Sm, Eu, Tb, Yb, Lu and Sc in two biological reference materials: NIST 1575 Pine Needles and BCR-CRM 101 Spruce Needles. The purpose was to contribute to the reference data for these two reference materials. The results were obtained with a good precision (relative standard deviations less than 15%). For the Pine Needles reference material there are already some proposed values and our results showed, in general, a good agreement with the data published. The contribution of uranium fission products to La, Ce, Nd and Sm was evaluated and considered in the determination of these elements. Interferences in the determination of rare earth elements in biological materials are also discussed. (author)

Reference methods and materials. A programme of support for regional and global marine pollution assessments

International Nuclear Information System (INIS)

1990-01-01

This document describes a programme of comprehensive support for regional and global marine pollution assessments developed by the United Nations Environment Programme (UNEP) in cooperation with the International Atomic Energy Agency (IAEA) and the Intergovernmental Oceanographic Commission (IOC) and with the collaboration of a number of other United Nations Specialized agencies including the Food and Agriculture Organisation (FAO), the World Meteorological Organisation (WMO), the World Health Organisation (WHO) and the International Maritime Organisation (IMO). Two of the principle components of this programme, Reference Methods and Reference materials are given special attention in this document and a full Reference Method catalogue is included, giving details of over 80 methods currently available or in an advanced stage of preparation and testing. It is important that these methods are seen as a functional component of a much wider strategy necessary for assuring good quality and intercomparable data for regional and global pollution monitoring and the user is encouraged to read this document carefully before employing Reference Methods and Reference Materials in his/her laboratory. 3 figs

Consensus values for NIST biological and environmental Standard Reference Materials

International Nuclear Information System (INIS)

Roelandts, I.; Gladney, E.S.

1998-01-01

The National Institute of Standards and Technology (NIST, formerly the National Bureau of Standards or NBS) has produced numerous Standard Reference Materials (SRM) for use in biological and environmental analytical chemistry. The value listed on the ''NIST Certificate of Analysis'' is the present best estimate of the ''true'' concentration of that element and is not expected to deviate from that concentration by more than the stated uncertainty. However, NIST does not certify the elemental concentration of every constituent and the number of elements reported in the NIST programs tends to be limited.Numerous analysts have published concentration data on these reference materials. Major journals in analytical chemistry, books, proceedings and ''technical reports'' have been surveyed to collect these available literature values. A standard statistical approach has been employed to evaluate the compiled data. Our methodology has been developed in a series of previous papers. Some subjective criteria are first used to reject aberrant data. Following these eliminations, an initial arithmetic mean and standard deviation (S.D.) are computed from remaining data for each element. All data now outside two S.D. from the initial mean are dropped and a second mean and S.D. recalculated. These final means and associated S.D. are reported as ''consensus values'' in our tables. (orig.)

Finding the joker among the maize endogenous reference genes for genetically modified organism (GMO) detection.

Science.gov (United States)

Paternò, Annalisa; Marchesi, Ugo; Gatto, Francesco; Verginelli, Daniela; Quarchioni, Cinzia; Fusco, Cristiana; Zepparoni, Alessia; Amaddeo, Demetrio; Ciabatti, Ilaria

2009-12-09

The comparison of five real-time polymerase chain reaction (PCR) methods targeted at maize ( Zea mays ) endogenous sequences is reported. PCR targets were the alcohol dehydrogenase (adh) gene for three methods and high-mobility group (hmg) gene for the other two. The five real-time PCR methods have been checked under repeatability conditions at several dilution levels on both pooled DNA template from several genetically modified (GM) maize certified reference materials (CRMs) and single CRM DNA extracts. Slopes and R(2) coefficients of all of the curves obtained from the adopted regression model were compared within the same method and among all of the five methods, and the limit of detection and limit of quantitation were analyzed for each PCR system. Furthermore, method equivalency was evaluated on the basis of the ability to estimate the target haploid genome copy number at each concentration level. Results indicated that, among the five methods tested, one of the hmg-targeted PCR systems can be considered equivalent to the others but shows the best regression parameters and a higher repeteability along the dilution range. Thereby, it is proposed as a valid module to be coupled to different event-specific real-time PCR for maize genetically modified organism (GMO) quantitation. The resulting practicability improvement on the analytical control of GMOs is discussed.

Using robust statistics to improve neutron activation analysis results

International Nuclear Information System (INIS)

Zahn, Guilherme S.; Genezini, Frederico A.; Ticianelli, Regina B.; Figueiredo, Ana Maria G.

2011-01-01

Neutron activation analysis (NAA) is an analytical technique where an unknown sample is submitted to a neutron flux in a nuclear reactor, and its elemental composition is calculated by measuring the induced activity produced. By using the relative NAA method, one or more well-characterized samples (usually certified reference materials - CRMs) are irradiated together with the unknown ones, and the concentration of each element is then calculated by comparing the areas of the gamma ray peaks related to that element. When two or more CRMs are used as reference, the concentration of each element can be determined by several different ways, either using more than one gamma ray peak for that element (when available), or using the results obtained in the comparison with each CRM. Therefore, determining the best estimate for the concentration of each element in the sample can be a delicate issue. In this work, samples from three CRMs were irradiated together and the elemental concentration in one of them was calculated using the other two as reference. Two sets of peaks were analyzed for each element: a smaller set containing only the literature-recommended gamma-ray peaks and a larger one containing all peaks related to that element that could be quantified in the gamma-ray spectra; the most recommended transition was also used as a benchmark. The resulting data for each element was then reduced using up to five different statistical approaches: the usual (and not robust) unweighted and weighted means, together with three robust means: the Limitation of Relative Statistical Weight, Normalized Residuals and Rajeval. The resulting concentration values were then compared to the certified value for each element, allowing for discussion on both the performance of each statistical tool and on the best choice of peaks for each element. (author)

230Th-234U Model-Ages of Some Uranium Standard Reference Materials

International Nuclear Information System (INIS)

Williams, R.W.; Gaffney, A.M.; Kristo, M.J.; Hutcheon, I.D.

2009-01-01

The 'age' of a sample of uranium is an important aspect of a nuclear forensic investigation and of the attribution of the material to its source. To the extent that the sample obeys the standard rules of radiochronometry, then the production ages of even very recent material can be determined using the 230 Th- 234 U chronometer. These standard rules may be summarized as (a) the daughter/parent ratio at time=zero must be known, and (b) there has been no daughter/parent fractionation since production. For most samples of uranium, the 'ages' determined using this chronometer are semantically 'model-ages' because (a) some assumption of the initial 230 Th content in the sample is required and (b) closed-system behavior is assumed. The uranium standard reference materials originally prepared and distributed by the former US National Bureau of Standards and now distributed by New Brunswick Laboratory as certified reference materials (NBS SRM = NBL CRM) are good candidates for samples where both rules are met. The U isotopic standards have known purification and production dates, and closed-system behavior in the solid form (U 3 O 8 ) may be assumed with confidence. We present here 230 Th- 234 U model-ages for several of these standards, determined by isotope dilution mass spectrometry using a multicollector ICP-MS, and compare these ages with their known production history

The use of reference materials in the elemental analysis of biological samples

International Nuclear Information System (INIS)

Bowen, H.J.M.

1975-01-01

Reference materials (RMs) are useful to compare the accuracy and precision of laboratories and techniques. The desirable properties of biological reference materials are listed, and the problems of production, homogenization and storage described. At present there are only 10 biological RMs available compared with 213 geological and 520 metallurgical RMs. There is a need for more biological RMs including special materials for microprobe analysis and for in vivo activation analysis. A study of 650 mean values for elements in RM Kale, analysed by many laboratories, leads to the following conclusions. 61% of the values lie within +-10% of the best mean, and 80% lie within +-20% of the best mean. Atomic absorption spectrometry gives results that are 5-30% high for seven elements, while intrumental neutron activation analysis gives low and imprecise results for K. Other techniques with poor interlaboratory precision include neutron activation for Mg, polarography for Zn and arc-spectrometry for many elements. More than half the values for elements in Kale were obtained by neutron activation, confirming the importance of this technique and the need for RMs. As a rough estimate, 6 x 10 9 elemental analyses of biological materials are carried out each year, mostly by medical, agricultural and food scientists. It seems likely that a substantial percentage of these are inaccurate, a situation that might be improved by quality control using standard RMs. (author)

Report of the 2nd research co-ordination meeting on reference materials for microanalytical nuclear techniques

International Nuclear Information System (INIS)

2002-01-01

Many microanalytical procedure require specific natural-matrix reference materials containing very low levels of trace elements and having a high degree of homogeneity. This proposed CRP will specifically address the question of quality control materials for these techniques. The participants of the meeting discussed the requirements for certified reference materials to by used in microanalysis with particular emphasis on the homogeneity issues. This publication contains summary of the discussions along with conclusions and recommendations made by the participants. The publication also contains ten individual presentations delivered by the participants. Each of the individual papers has been provided with an abstract and indexed separately

Austenitic chromium nickel steel as standard reference material in measurement of thermal and temperature conductivity

International Nuclear Information System (INIS)

Binkele, L.

1990-01-01

A niobium-stabilized CrNi steel with the NBS designation SRM 735 is introduced as WLF standard reference material in a report by Hust and Giarratano, for the temperature range 300-1200 K and for thermal conductivities around 20 W/mk. However, its specification does not show it to be a direct member of the DIN family of CrNi steels. This report should be regarded as a continuation and supplement to the above-mentioned efforts in America. On the one hand, a solution of a possibly too-narrow specification is aimed at for the reference material, where it is important how sensitive the thermal conductivity is to changes in the chemical composition and changes of the manufacturing parameters and what accuracy can be reached for the reference values with the best measurement techniques. On the other hand, the data base should be expanded and the accuracy of the reference curve should be improved if possible. (orig./MM) [de

Reference Materials for Calibration of Analytical Biases in Quantification of DNA Methylation.

Science.gov (United States)

Yu, Hannah; Hahn, Yoonsoo; Yang, Inchul

2015-01-01

Most contemporary methods for the quantification of DNA methylation employ bisulfite conversion and PCR amplification. However, many reports have indicated that bisulfite-mediated PCR methodologies can result in inaccurate measurements of DNA methylation owing to amplification biases. To calibrate analytical biases in quantification of gene methylation, especially those that arise during PCR, we utilized reference materials that represent exact bisulfite-converted sequences with 0% and 100% methylation status of specific genes. After determining relative quantities using qPCR, pairs of plasmids were gravimetrically mixed to generate working standards with predefined DNA methylation levels at 10% intervals in terms of mole fractions. The working standards were used as controls to optimize the experimental conditions and also as calibration standards in melting-based and sequencing-based analyses of DNA methylation. Use of the reference materials enabled precise characterization and proper calibration of various biases during PCR and subsequent methylation measurement processes, resulting in accurate measurements.

Stability of aflatoxin B1 in animal feed candidate reference materials

NARCIS (Netherlands)

Roos, A.H.; Mazijk, van R.J.; Tuinstra, L.G.M.T.; Huf, F.A.

1991-01-01

Two candidate reference materials animal feed were stored at a temperature of -18°C, 4 C, 20°C and 37°C. The stability of aflatoxin B1 was studied duringa period of two years. A significant decrease in the aflatoxin B1 content was measured in the samples stared at 20°C and 37°C. In the samples

Grain-size effects on PIXE and INAA analysis of IAEA-336 lichen reference material

Science.gov (United States)

Marques, A. P.; Freitas, M. C.; Wolterbeek, H. Th.; Verburg, T. G.; De Goeij, J. J. M.

2007-02-01

IAEA-336 lichen certified reference material was used to compare outcomes from INAA and PIXE elemental analyses, in relationship with grain size. The IAEA material (grain size lichen reference material's particle size distribution follows a bimodal distribution, which is turning more and more monomodal after further fine sieving. Replicates of each fraction were analysed by INAA and PIXE. Results for Cl, K, Mn, Fe and Zn by both techniques were compared by application of z-values tested against the criterion ∣ z∣ limited amount of lichen material as "seen" in the PIXE analysis and the grain size distribution in the lichen material were no causes of measurable differences between the results of both techniques. However, fractionation into smaller grain sizes showed to be associated with lower element content, for Na, Cl, K, Mn and Sr even up to a factor of 2. The observed increases of the proportion of algae in the smaller grain-size fractions and the possible accumulation capacity for certain elements in the fungal part of the lichen may explain the observed phenomenon. The sieving process and consequently the discarding of part of the material have lead to a change of the properties of the original sample, namely algae/fungus percentage and elemental contents.

A feasibility study for producing an egg matrix candidate reference material for the polyether ionophore salinomycin.

Science.gov (United States)

Ferreira, Rosana Gomes; Monteiro, Mychelle Alves; Pereira, Mararlene Ulberg; da Costa, Rafaela Pinto; Spisso, Bernardete Ferraz; Calado, Veronica

2016-08-01

The aim of this work was to study the feasibility of producing an egg matrix candidate reference material for salinomycin. Preservation techniques investigated were freeze-drying and spray drying dehydration. Homogeneity and stability studies of the produced batches were conducted according to ISO Guides 34 and 35. The results showed that all produced batches were homogeneous and both freeze-drying and spray drying techniques were suitable for matrix dehydrating, ensuring the material stability. In order to preserve the material integrity, it must be transported within the temperature range of -20 up to 25°C. The results constitute an important step towards the development of an egg matrix reference material for salinomycin is possible. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of cadmium, lead and zinc in a candidate reference materials using isotope dilution mass spectrometry

International Nuclear Information System (INIS)

Munoz, Luis; Gras, Nuri; Quejido, Alberto; Fernandez, Marta

2001-01-01

The growing demands placed on analytical laboratories to ensure the reliability of their results, due to the introduction of systems of quality and to the increasing use of metrology in chemical measurements has led most laboratories to validate their methodologies and to control them statistically. One of the techniques used most often for these purposes is based on the use of reference materials. The proper use of these materials means that laboratory results may be traced to the International System of Units, analytical methodologies can be validated, instruments calibrated and chemical measurements harmonized. One of the biggest challenges in developing reference materials is that of certifying their properties, a process that has been defined as assigning a concentration value that is as close as possible to the true value together with its uncertainty. Organizations that produce reference materials use several options for their certification process, and among these is the use of a primary method. Among the primary methods recognized by the International Office of Weights and Measures is the Isotope Dilution Mass Spectrometry technique. The Chilean Nuclear Energy Commission, through its Reference Materials Program, has prepared a reference material of clam tissue, which has been chemically defined by different analytical methodologies applied in different national and international laboratories. This work describes the methodology developed with the CIEMAT for determining the elements lead, cadmium and zinc in the clam tissue reference material using the primary technique of Isotope Dilution Mass Spectrometry. The calculation is described for obtaining the spike amounts to be added to the sample and the procedure is explained for carrying out the isotopic exchange. The isotopic relationships 204 Pb/ 205 Pb, 111 Cd/ 114 Cd and 66 Zn/ 67 Zn were determined in an atomic emission spectrometer with a plasma source with the following characteristics: plasma

Development of saw palmetto (Serenoa repens) fruit and extract standard reference materials.

Science.gov (United States)

Schantz, Michele M; Bedner, Mary; Long, Stephen E; Molloy, John L; Murphy, Karen E; Porter, Barbara J; Putzbach, Karsten; Rimmer, Catherine A; Sander, Lane C; Sharpless, Katherine E; Thomas, Jeanice B; Wise, Stephen A; Wood, Laura J; Yen, James H; Yarita, Takashi; NguyenPho, Agnes; Sorenson, Wendy R; Betz, Joseph M

2008-10-01

As part of a collaboration with the National Institutes of Health's Office of Dietary Supplements and the Food and Drug Administration's Center for Drug Evaluation and Research, the National Institute of Standards and Technology has developed two standard reference materials (SRMs) representing different forms of saw palmetto (Serenoa repens), SRM 3250 Serenoa repens fruit and SRM 3251 Serenoa repens extract. Both of these SRMs have been characterized for their fatty acid and phytosterol content. The fatty acid concentration values are based on results from gas chromatography with flame ionization detection (GC-FID) and mass spectrometry (GC/MS) analysis while the sterol concentration values are based on results from GC-FID and liquid chromatography with mass spectrometry analysis. In addition, SRM 3250 has been characterized for lead content, and SRM 3251 has been characterized for the content of beta-carotene and tocopherols. SRM 3250 (fruit) has certified concentration values for three phytosterols, 14 fatty acids as triglycerides, and lead along with reference concentration values for four fatty acids as triglycerides and 16 free fatty acids. SRM 3251 (extract) has certified concentration values for three phytosterols, 17 fatty acids as triglycerides, beta-carotene, and gamma-tocopherol along with reference concentration values for three fatty acids as triglycerides, 17 fatty acids as free fatty acids, beta-carotene isomers, and delta-tocopherol and information values for two phytosterols. These SRMs will complement other reference materials currently available with concentrations for similar analytes and are part of a series of SRMs being developed for dietary supplements.

NBS SRM 1569 Brewer's Yeast: Is it an adequate standard reference material for testing a chromium determination in biological materials tion in biological materials

International Nuclear Information System (INIS)

Goeij, J.J.M. de; Volkers, K.J.; Tjioe, P.S.; Kroon, J.J.

1978-01-01

Some analytical experiences with NBS SRM 1569 Brewer's Yeast are presented. Against this background the adequacy of this standard reference material for the determination of chromium in biological materials is discussed. Authors have three main objections. Due to its high content of insoluble chromium-containing particles, SRM 1569 is not typical for biological materials, possibly not even for Brewer's Yeast. The chromium level of SRM 1569 is not typical for the chromium levels normally encountered in pure biological materials. The major fraction (69 +- 3 percent) of the chromium is present in a form which is insoluble under the conditions used in Author's analysis. (T.I.)

Certification of a plutonium dioxide reference material for elemental analyses (EC-NRM 210)

International Nuclear Information System (INIS)

Le Duigou, Y.

1990-01-01

A new EC plutonium reference material is made available in the form of 5g samples of plutonium dioxide powder. Before weighing the material must be calcined at 1 250 0 C for two hours. The plutonium content (880.26 ± 0.44) g.kg -1 has been derived from plutonium measurements performed by three different laboratories each applying a different oxydo-reductive method. The results of the plutonium measurement, the statistical evaluation of the uncertainty of the plutonium content together with information on the impurities present in the material are given in the report

Development of in-plant reference material for composition of chinese cabbage with certified selenium content

Directory of Open Access Journals (Sweden)

D. A. Chupahin

2014-01-01

Full Text Available In-plant reference material for composition of Chinese cabbage with certified selenium content was developed for accuracy control of the results of selenium determination and within-laboratory quality control of analytical work in the analysis of food raw material.

Certification of biological reference materials: participation of the Neutron Activation Laboratory (LAN-IPEN/CNEN-SP)

International Nuclear Information System (INIS)

Ticianelli, Regina B.; Figueiredo, Ana Maria G.

2007-01-01

Analytical laboratories have as one of their important goals to demonstrate their competence allowing international acceptance and comparison of analytical data. The IPEN Neutron Activation Laboratory (LAN-IPEN) has implemented its Quality Assurance Program which comprises, among other activities, the participation in intercomparison runs. As a part of this Quality Assurance Program, LAN-IPEN has participated in interlaboratorial trials to analyze two biological candidate reference materials: INCT-CF-3 Corn Flour and INCT-SBF-4 Soya Bean Flour from the Institute of Nuclear Chemistry And Technology (Warszawa, Poland). The elements Br, Ca, Co, Cs, Fe, K, Na, Rb and Zn were analyzed in the candidate reference materials by instrumental neutron activation analysis (INAA). The performance of the laboratory was statistically evaluated in relation to the consensus values for these materials using the Z-Score test. This laboratory evaluation method has been accepted as a standard by ISO/IUPAC. In the present study, adequate Z-Score values (|Z|<2) were observed for all of the analyzed elements, confirming the accuracy of the nuclear methodology employed. The contribution of LAN-IPEN in the certification of the reference materials analyzed was very important, since the results provided were used in the statistical evaluation of the certified value. (author)

Development of Candidate Reference Materials of Endosulfan Sulfate and Bifenthrin in Black Tea

Directory of Open Access Journals (Sweden)

Nurhani Aryana

2016-03-01

Full Text Available The candidate reference materials of endosulfan sulfate and bifenthrin in black tea have been developed according to the requirements of ISO Guide 34 and 35. Preparation of candidate material includes grinding and sieving of the black tea leaves, spiking the black tea powder by both analytes, homogenization, and bottling. Homogeneity and short-term stability test were performed using a GC-µECD instrument. Meanwhile, the characterization was carried out by a collaborative study using both of GC-µECD and GC-MS instruments. The uncertainty budget was evaluated from sample inhomogeneity, short-term instability and variability in the characterization procedure. In a dry mass fraction, endosulfan sulfate was assigned to be 491 µg kg-1 with a relative expanded uncertainty of ± 33.2%, and bifenthrin was assigned to be 937 µg kg-1 with a relative expanded uncertainty of ± 18.5%. The candidate reference materials are aimed to support the need of matrix CRM especially for the measurement of pesticide residue for quality assurance work done by laboratories in Indonesia.

Quantification of the predominant monomeric catechins in baking chocolate standard reference material by LC/APCI-MS.

Science.gov (United States)

Nelson, Bryant C; Sharpless, Katherine E

2003-01-29

Catechins are polyphenolic plant compounds (flavonoids) that may offer significant health benefits to humans. These benefits stem largely from their anticarcinogenic, antioxidant, and antimutagenic properties. Recent epidemiological studies suggest that the consumption of flavonoid-containing foods is associated with reduced risk of cardiovascular disease. Chocolate is a natural cocoa bean-based product that reportedly contains high levels of monomeric, oligomeric, and polymeric catechins. We have applied solid-liquid extraction and liquid chromatography coupled with atmospheric pressure chemical ionization-mass spectrometry to the identification and determination of the predominant monomeric catechins, (+)-catechin and (-)-epicatechin, in a baking chocolate Standard Reference Material (NIST Standard Reference Material 2384). (+)-Catechin and (-)-epicatechin are detected and quantified in chocolate extracts on the basis of selected-ion monitoring of their protonated [M + H](+) molecular ions. Tryptophan methyl ester is used as an internal standard. The developed method has the capacity to accurately quantify as little as 0.1 microg/mL (0.01 mg of catechin/g of chocolate) of either catechin in chocolate extracts, and the method has additionally been used to certify (+)-catechin and (-)-epicatechin levels in the baking chocolate Standard Reference Material. This is the first reported use of liquid chromatography/mass spectrometry for the quantitative determination of monomeric catechins in chocolate and the only report certifying monomeric catechin levels in a food-based Standard Reference Material.

Value determination of ZrO2 in-house reference material (RM) candidate

International Nuclear Information System (INIS)

Susanna Tuning Sunanti; Samin; Supriyanto C

2013-01-01

The value determination of zirconium oxide in-house reference materials (RM) candidate has been done by referring to ISO:35-2006 standard. The raw material of RM was 4 kg of ZrO 2 , Merck, that was dried at 90°C for 2×6 hours in a closed room. The samples were crushed with stainless steel (SS) pestle to pass ≤ 200 mesh sieve, homogenized in a homogenizer for 3×6 hours to obtain the powdered, dried and homogenous samples. The gravimetric method was performed to test the moisture content, while XRF and AAS methods were used to test the homogeneity and stability of samples candidates. Reference material (RM) candidates of ZrO 2 powder were put into polyethylene bottles, each weighing 100 g. Samples were distributed to 10 testing laboratories that have been accredited for testing the composition of the oxide contents and loss of ignition (LOI) using variety of analytical methods that have been validated such as AAS, XRF, NAA, and UV-Vis. The testing results of oxide content and loss of ignition parameters from various laboratories were analyzed using statistical methods. The testing data of oxide concentration in zirconium oxide RM candidates obtained from various laboratories were ZrO 2 : 97.7334 ± 0.0016%, HfO 2 : 1.7329 ± 0.0024%, SiO 2 : 30.1224 ± 0.0053%, Al 2 O 3 : 0.0245 ± 0.0015%, TiO 2 : 0.0153 ± 0.0006%, Fe 2 O 3 : 0.0068 ± 0.0005%, CdO: 3.1798 ± 0.00006 ppm, and the LOI results was = 0.0217 ± 0.00022%. (author)

Certified Reference Material IAEA-446 for radionuclides in Baltic Sea seaweed

DEFF Research Database (Denmark)

Pham, M.K.; Benmansour, M.; Carvalho, F.P.

2014-01-01

A Certified Reference Material (CRM) for radionuclides in seaweed (Fucus vesiculosus) from the Baltic Sea (IAEA-446) is described and the results of the certification process are presented. The 40K, 137Cs, 234U and 239þ240Pu radionuclides were certified for this material, and information values...... for 12 other radionuclides (90Sr, 99Tc, 210Pb (210Po), 226Ra, 228Ra, 228Th, 230Th, 232Th, 235U, 238U, 239Pu and 240Pu) are presented. The CRM can be used for Quality Assurance/Quality Control of analysis of radionuclides in seaweed and other biota samples, as well as for development and validation...

Nuclear microprobe analysis of the standard reference materials

International Nuclear Information System (INIS)

Jaksic, M.; Fazinic, S.; Bogdanovic, I.; Tadic, T.

2002-01-01

Most of the presently existing Standard Reference Materials (SRM) for nuclear analytical methods are certified for the analyzed mass of the order of few hundred mg. Typical mass of sample which is analyzed by PIXE or XRF methods is very often below 1 mg. By the development of focused proton or x-ray beams, masses which can be typically analyzed go down to μg or even ng level. It is difficult to make biological or environmental SRMs which can give desired homogeneity at such low scale. However, use of fundamental parameter quantitative evaluation procedures (absolute method), minimize needs for SRMs. In PIXE and micro PIXE setup at our Institute, fundamental parameter approach is used. For exact calibration of the quantitative analysis procedure just one standard sample is needed. In our case glass standards which showed homogeneity down to micron scale were used. Of course, it is desirable to use SRMs for quality assurance, and therefore need for homogenous materials can be justified even for micro PIXE method. In this presentation, brief overview of PIXE setup calibration is given, along with some recent results of tests of several SRMs

The use of high accuracy NAA for the certification of NIST botanical standard reference materials

International Nuclear Information System (INIS)

Becker, D.A.; Greenberg, R.R.; Stone, S.F.

1992-01-01

Neutron activation analysis is one of many analytical techniques used at the National Institute of Standards and Technology (NIST) for the certification of NIST Standard Reference Materials (SRMs). NAA competes favorably with all other techniques because of it's unique capabilities for high accuracy even at very low concentrations for many elements. In this paper, instrumental and radiochemical NAA results are described for 25 elements in two new NIST SRMs, SRM 1515 (Apple Leaves) and SRM 1547 (Peach Leaves), and are compared to the certified values for 19 elements in these two new botanical reference materials. (author) 7 refs.; 4 tabs

Report of the consultants' meeting on traceability of IAEA-AQCS reference materials to SI-units

International Nuclear Information System (INIS)

2002-01-01

The purpose of the meeting was to discuss the present Agency's Analytical Quality Control Services (AQCS) procedure for the characterization of reference materials and to identify necessary improvements or changes needed to fulfill the requirements on traceability and uncertainty related to the property value of IAEA reference materials. This publication contains a summary of the discussions held at the meeting as well as specific recommendations made by the consultants. It also contains draft reports of two previous meetings and individual papers presented by the consultants at the meeting. These reports and papers have been provided with abstracts and indexed separately

230Th-234U Model-Ages of Some Uranium Standard Reference Materials

Energy Technology Data Exchange (ETDEWEB)

Williams, R W; Gaffney, A M; Kristo, M J; Hutcheon, I D

2009-05-28

The 'age' of a sample of uranium is an important aspect of a nuclear forensic investigation and of the attribution of the material to its source. To the extent that the sample obeys the standard rules of radiochronometry, then the production ages of even very recent material can be determined using the {sup 230}Th-{sup 234}U chronometer. These standard rules may be summarized as (a) the daughter/parent ratio at time=zero must be known, and (b) there has been no daughter/parent fractionation since production. For most samples of uranium, the 'ages' determined using this chronometer are semantically 'model-ages' because (a) some assumption of the initial {sup 230}Th content in the sample is required and (b) closed-system behavior is assumed. The uranium standard reference materials originally prepared and distributed by the former US National Bureau of Standards and now distributed by New Brunswick Laboratory as certified reference materials (NBS SRM = NBL CRM) are good candidates for samples where both rules are met. The U isotopic standards have known purification and production dates, and closed-system behavior in the solid form (U{sub 3}O{sub 8}) may be assumed with confidence. We present here {sup 230}Th-{sup 234}U model-ages for several of these standards, determined by isotope dilution mass spectrometry using a multicollector ICP-MS, and compare these ages with their known production history.

The Kjeldahl method as a primary reference procedure for total protein in certified reference materials used in clinical chemistry. II. Selection of direct Kjeldahl analysis and its preliminary performance parameters.

Science.gov (United States)

Vinklárková, Bára; Chromý, Vratislav; Šprongl, Luděk; Bittová, Miroslava; Rikanová, Milena; Ohnútková, Ivana; Žaludová, Lenka

2015-01-01

To select a Kjeldahl procedure suitable for the determination of total protein in reference materials used in laboratory medicine, we reviewed in our previous article Kjeldahl methods adopted by clinical chemistry and found an indirect two-step analysis by total Kjeldahl nitrogen corrected for its nonprotein nitrogen and a direct analysis made on isolated protein precipitates. In this article, we compare both procedures on various reference materials. An indirect Kjeldahl method gave falsely lower results than a direct analysis. Preliminary performance parameters qualify the direct Kjeldahl analysis as a suitable primary reference procedure for the certification of total protein in reference laboratories.

Reference materials and measurement traceability

International Nuclear Information System (INIS)

Bingham, C.D.

1980-01-01

Nuclear materials safeguards within the U.S.A. are accomplished by the integration of activities involving physical protection, material control and material accountability. Material accountability requires both sound measurement technology and well-defined accounting procedures to provide final evidence that physical protection and materials control have achieved their purpose. 5 refs

Preparation, characterization and certification of uranium isotope reference materials

International Nuclear Information System (INIS)

Oliveira Junior, Olivio Pereira de

2006-01-01

This work describes the preparation, characterization and certification of a set of uranium isotope reference materials ranging from 0.5 to 20.0 % of 235 U in mass. The most important concepts of metrology in chemical measurements were applied so that the certified quantities in these materials could be directly traceable to the International System of Units (SI). As a consequence of this approach, these materials can be used in the instruments calibration, estimation of measurement uncertainty, method validation, assessment of performance of analysts, quality control routines and interlaboratory comparison programmes. The most advanced methods and techniques in mass spectrometry, that is, gas source mass spectrometry (GSMS), thermal ionisation mass spectrometry (TIMS) and inductively coupled plasma mass spectrometry (ICPMS) were investigated to identify which are the dominant components in the uncertainty and to quantify its contribution to the final value of the measurement uncertainty of the isotopic ratio. The results obtained were then compared to verify which are the methods and techniques associated to the lowest measurement uncertainty values. The isotope amount ratio n( 235 U)/n( 238 U) was certified in the materials produced to expanded uncertainties ranging from 0.02 to 0.10 % and the ratios n( 234 U)/n( 238 U) and n( 236 U)/n( 238 U), to uncertainties ranging from 0.03 to 2.20 %. These values fully comply to the requirements of the isotopic characterization of nuclear fuel as well as the analysis of environmental samples for nuclear safeguards. (author)

Neutron activation analysis for certification of standard reference materials

International Nuclear Information System (INIS)

Capote Rodriguez, G.; Perez Zayas, G.; Hernandez Rivero, A.; Ribeiro Guevara, S.

1996-01-01

Neutron activation analysis is used extensively as one of the analytical techniques in the certification of standard reference materials. Characteristics of neutron activation analysis which make it valuable in this role are: accuracy multielemental capability to asses homogeneity, high sensitivity for many elements, and essentially non-destructive method. This paper report the concentrations of 30 elements (major, minor and trace elements) in four Cuban samples. The samples were irradiated in a thermal neutron flux of 10 12- 10 13 n.cm 2. s -1. The gamma ray spectra were measured by HPGe detectors and were analyzed using ACTAN program development in Center of Applied Studies for Nuclear Development

Development of the NBS beryllium isotopic standard reference material

International Nuclear Information System (INIS)

Inn, K.G.W; Fassett, J.D.; Coursey, B.M.; Walker, R.L.; Raman, S.

1987-01-01

The National Bureau of Standards, in conjunction with the Oak Ridge National Laboratory and the Accelerator Mass Spectrometry community, is in the process of developing a beryllium isotopic solution Standard Reference Material. The master 10 Be/ 9 Be solution was characterized isotopically by resonance-ionization and secondary-ion mass-spectrometric-based techniques, and radioactivity measurements were by liquid scintillation counting. The master solution was gravimetrically diluted with 9 Be to a final 10 Be/ 9 Be atomic ratio of 3 x 10 -11 . The preliminary data indicate a half life for 10 Be of 1.3 million years, and AMS measurements are within 10% of the known beryllium isotopic ratio

Certification of standard reference materials employing neutron activation analysis

International Nuclear Information System (INIS)

Capote Rodriguez, G.; Hernandez Rivero, A.; Molina Insfran, J.; Ribeiro Guevara, S.; Santana Encinosa, C.; Perez Zayas, G.

1997-01-01

Neutron activation analysis (Naa) is used extensively as one of the analytical techniques in the certification of standard reference materials (Srm). Characteristics of Naa which make it valuable in this role are: accuracy; multielemental capability; ability to assess homogeneity; high sensitivity for many elements, and essentially non-destructive method. This paper reports the concentrations of thirty elements (major, minor and trace elements) in four Cuban Srm's. The samples were irradiated in a thermal neutron flux of 10 12 -10 13 neutrons.cm -2 .s -1 . The gamma-ray spectra were measured by HPGe detectors and were analysed using ACTAN program, developed in CEADEN. (author) [es

Prepare of microanalysis reference material for nuclear analysis of Chinese ancient ceramic

International Nuclear Information System (INIS)

Feng Songlin; Xu Qing; Feng Xiangqian; Fan Dongyu; Lei Yong; Cheng Lin

2005-01-01

Some analytic technique can play important role for identifying the provenance and age of ceramic ware. However, it is usually not allowed to destructive analyze for a valuable intact porcelain ware. These analysis methods such as X-ray Fluorescence (XRF), Proton Induced X-ray Emission (PIXE), and Synchrotron Radiation X-ray Fluorescence (SRXRF) are suitable for nondestructive analysis of ancient ceramic wares. In order to compare the analytic data obtained by different measuring method and identify the provenance and age accurately, the effective way is to calibrate elemental concentration in body and glaze of ceramic ware. Microanalysis reference material (MRM) of ancient ceramic has to be prepared for achieving quantitative analysis. A solid powder 99% in size of 500 mesh for microanalysis reference material (MRM) has being prepared in institute of high energy physics. The minimum analytic masses of 1 mg were determined by Neutron Activation Analysis (NAA) for these elements (Sc, Cr, Co, Rb: Cs, La, Ce, Nd, Sm, Tb, Yb, Lu; Hf, Ta, Th, U), and by SRXRF for elements (K, Ca, Ti, Mn, Fe, Zn; Rb, Sr).

The influence of different referencing methods on the accuracy of δ(13) C value measurement of ethanol fuel by gas chromatography/combustion/isotope ratio mass spectrometry.

Science.gov (United States)

Neves, Laura A; Rodrigues, Janaína M; Daroda, Romeu J; Silva, Paulo R M; Ferreira, Alexandre A; Aranda, Donato A G; Eberlin, Marcos N; Fasciotti, Maíra

2015-11-15

Brazil is the largest producer of sugar cane bioethanol in the world. Isotope ratio mass spectrometry (IRMS) is the technique of choice to certify the origin/raw materials for ethanol production, but the lack of certified reference materials (CRMs) for accurate measurements of δ(13) C values traceable to Vienna Pee Dee Belemnite (VPDB), the international zero point for (13) C/(12) C measurements, certified and compatible with gas chromatography (GC)/IRMS instruments may compromise the accuracy of δ(13) C determinations. We evaluated the influence of methods for the calibration and normalization of raw δ(13) C values of ethanol samples. Samples were analyzed by GC/C/IRMS using two different GC columns. Different substances were used as isotopic standards for the working gas calibration. The δ(13) C values obtained with the three methods of normalization were statistically compared with those obtained with elemental analyzer (EA)/IRMS, since the δ(13) C results obtained using EA are traceable to VPDB via the NBS 22 reference material. It was observed that both the isotopic reference material for CO2 calibration and the GC column have a major effect on the δ(13) C measurements, leading to a bias of almost 2-3 ‰ in the δ(13) C values. All three methods of normalization were equivalent in performance, enabling an improvement in the GC/C/IRMS accuracy, compared with the EA/IRMS reference values for the samples. All the methods of CO2 calibration, chromatography and normalization presented in this work demonstrated several sources of traceability and accuracy loss for the determination of δ(13) C values in ethanol fuel samples by GC/C/IRMS. This work has also shown the importance of using proper CRMs traceable to VPBD that should be compatible and certified using GC/C/IRMS, ideally in a wide range of δ(13) C values. This is important not only for bioethanol fuel samples, but also for many analytes commonly analyzed by IRMS. Copyright © 2015 John Wiley & Sons

Performance of NAA methods in an International Interlaboratory Reference Material Characterization Campaign

International Nuclear Information System (INIS)

Ihnat, M.

2000-01-01

An extensive database of analytical results from a recent biological matrix Reference Material Characterization Campaign permitted an intercomparison of the performances of various methods among each other and with 'true' best estimate concentration values established for these materials. Six different variants of neutron activation analysis (NAA) methods were employed including: instrumental neutron activation analysis, instrumental neutron activation analysis with acid digestion, neutron activation analysis with radiochemical separation, neutron capture prompt gamma activation analysis, epithermal instrumental neutron activation analysis, and neutron activation analysis with preconcentration. The precision and accuracy performance of NAA-based analytical methods are compared with three other major techniques, atomic absorption spectrometry (AAS), atomic emission spectrometry (AES) and mass spectrometry (MS) for 28 elements in 10 natural matrix materials. (author)

Preparation and certification of Re-Os dating reference materials: Molybdenites HLP and JDC

Science.gov (United States)

Du, A.; Wu, S.; Sun, D.; Wang, Shaoming; Qu, W.; Markey, R.; Stain, H.; Morgan, J.; Malinovskiy, D.

2004-01-01

Two Re-Os dating reference material molybdenites were prepared. Molybdenite JDC and molybdenite HLP are from a carbonate vein-type molybdenum-(lead)- uranium deposit in the Jinduicheng-Huanglongpu area of Shaanxi province, China. The samples proved to be homogeneous, based on the coefficient of variation of analytical results and an analysis of variance test. The sampling weight was 0.1 g for JDC and 0.025 g for HLP. An isotope dilution method was used for the determination of Re and Os. Sample decomposition and preconcentration of Re and Os prior to measurement were accomplished using a variety of methods: acid digestion, alkali fusion, ion exchange and solvent extraction. Negative thermal ionisation mass spectrometry and inductively coupled plasma-mass spectrometry were used for the determination of Re and 187Os concentration and isotope ratios. The certified values include the contents of Re and Os and the model ages. For HLP, the Re content was 283.8 ?? 6.2 ??g g-1, 187Os was 659 ?? 14 ng g-1 and the Re-Os model age was 221.4 ?? 5.6 Ma. For JDC, the Re content was 17.39 ?? 0.32 ng g-1, 187Os was 25.46 ?? 0.60 ng g-1 and the Re-Os model age was 139.6 ?? 3.8 Ma. Uncertainties for both certified reference materials are stated at the 95% level of confidence. Three laboratories (from three countries: P.R. China, USA, Sweden) joined in the certification programme. These certified reference materials are primarily useful for Re-Os dating of molybdenite, sulfides, black shale, etc.

Preparação de um material de referência certificado para controle de agrotóxicos em hortifrutigranjeiros: estudo da homogeneidade Preparation of a certified reference material for pesticide control in the cultivation of fruits and vegetables: a homogeneity study

Directory of Open Access Journals (Sweden)

Maria Helena Wohlers Morelli Cardoso

2010-06-01

Full Text Available Neste trabalho são apresentados os esforços para garantir a homogeneidade de um material de referência. Níveis residuais (mg.kg-1 de quatro agrotóxicos (γ-HCH, fenitrotiona, clorpirifós e procimidona foram adicionados à polpa de tomate com o objetivo de se preparar um material de referência certificado. As propriedades mais importantes desses materiais são a homogeneidade e a estabilidade. Antes de serem enviados a outros laboratórios, os materiais de referência precisam ter sua homogeneidade verificada. Nas etapas prévias, amostras foram avaliadas de modo a prover dados sobre o tratamento mais adequado para minimizar a variabilidade analítica do lote preparado e garantir a qualidade da amostra candidata a material de referência certificado, tão bem como a estimativa da incerteza associada à homogeneidade. A análise de variância fornece informações sobre a variabilidade do lote preparado e o grau de invariabilidade da amostra fortificada. Depois da preparação, as amostras foram expostas à radiação gama na dose de 2 kGy e submetidas a um estudo interlaboratorial para certificação. As concentrações certificadas dos agrotóxicos após caracterização foram 0,191 ± 0,047 mg.kg-1; 0,192 ± 0,068 mg.kg-1; 0,225 ± 0,076 mg.kg-1e 0,177 ± 0,051 mg.kg-1 para o γ-HCH, a fenitrotiona, clorpirifós e procimidona respectivamente.This study reports on the efforts to ensure homogeneity of certified reference materials. Residues of four pesticides (γ-HCH, fenitrothion, chlorpyrifos, and procymidone were added to tomato pulp in order to produce reference materials. The two most important properties of such materials are known to be homogeneity and stability. Before being shipped to other laboratories, reference materials must have their homogeneity certified. As part of a preliminary study, hundreds of samples were investigated in order to provide data on the most suitable treatments to minimize analytical variability and

Intercomparison of enriched stable isotope reference materials for medical and biological studies

International Nuclear Information System (INIS)

Parr, R.M.; Clements, S.A.

1991-01-01

This report summarizes the results of an intercomparison exercise organized by the IAEA during the latter part of 1988 and 1989. Data are presented for 13 different kinds of enriched stable isotope reference material containing 2 H, 13 C, 15 N and 18 O. Results were submitted by forty participants in twenty countries. 2 refs, 13 figs, 18 tabs

An independent accurate reference method for the determination of chromium in biological materials

NARCIS (Netherlands)

Lagerwaard, A.; Woittiez, J.R.W.; de Goeij, J.J.M.

1994-01-01

A method for the determination of Cr in biological materials with high accuracy is reported for use as an independent reference method. It is based on radiochemical neutron activation analysis (RNAA) in combination with an individual yield determination based on the online yield principle. A

Reference material for trace analysis by radioanalytical methods: Bowen's Kale

International Nuclear Information System (INIS)

Wainerdi, R.E.

1979-01-01

A fairly large volume of published data on 'Bowen's Kale' has been examined critically in order to develop recommendations for the use of this preparation as a 'reference material' in the standardisation and evaluation of the reliability of analytical procedures. Values are now recommended for the contents of twelve elements present in major to trace concentrations in 'Bowen's Kale'. 'Indicated values' for another 16 elements are provided. Values for 15 more elements are listed with no recommendation. The criteria adopted in categorising elements into these groups are discussed. (author)

Nanogram determination of arsenic in biological reference materials by non-destructive Compton suppression neutron activation analysis

International Nuclear Information System (INIS)

Petra, M.; Landsberger, S.; Swift, G.

1990-01-01

Non-destructive epithermal neutron activation analysis in conjunction with Compton suppression has been applied to determine arsenic in seven biological standard reference materials from the National Institute of Standards and Technology. The accuracy is in excellent agreement with all the certified values and compilation results. For four of the materials detection limits between 1-4 ng/g were easily achieved while for three others they ranged from 18-50 ng/g. Overall analytical precision typically varied between 2-4% for five of the reference materials while for two other it was between 12-16%. These methods clearly demonstrate that through a judicious approach of anti-coincidence techniques, nanogram quantities of arsenic can be reliably determined without the need for labor intensive chemical separations. (orig.)

The production and certification of a plutonium equal-atom reference material: NBL CRM 128

International Nuclear Information System (INIS)

Crawford, D.W.

1990-07-01

This report describes the design, production, and certification of the New Brunswick Laboratory plutonium equal-atom certified reference material (CRM), NBL CRM 128. The primary use of this CRM is for the determination of bias corrections encountered in the operation of a mass spectrometer. This reference material is available to the US Department of Energy contractor-operated and government-operated laboratories, as well as to the international nuclear safeguards community. The absolute, or unbiased, certified value for the CRM's Pu-242/Pu-239 ratio is 1.00063 ± 0.00026 (95% confidence interval) as of October 1, 1984. This value was obtained through the quantitative blending of high-purity, chemically and isotopically characterized separated isotopes, as well as through intercomparisons of CRM samples with calibration mixtures using thermal ionization mass spectrometry. 32 tabs

Ways for accurate analysis of high purity materials using the glow discharge mass spectrometry (GD-MS); Wege zur genauen Charakterisierung hochreiner Materialien mit der Glimmentladungs-Massenspektrometrie (GD-MS)

Energy Technology Data Exchange (ETDEWEB)

Gusarova, Tamara

2010-04-14

The main aim of this work consists in the investigation, development and application of improved possibilities of accurate analysis of high purity materials using the solid sample technique of Glow Discharge Mass Spectrometry (GD-MS), as well as in the sensitivity enhancement of GD Optical Emission Spectrometry (GD-OES) by implicating the hollow cathode effect. The emphasis of the PhD thesis consists in the accurate quantification for GD-MS. As appropriate certified reference materials (CRMs) for calibration are lacking in most cases an accurate quantification especially for trace elements mass fractions at {mu}g kg{sup -1} level can often not be achieved. To overcome this problem and to expand the possibilities of modern GD-MS hereby, synthetic standards were applied for calibration of both high resolution GD-MS instruments ''VG 9000'' and ''Element GD''. The standards were prepared by doping of matrix powder with trace element standard solutions followed by drying and pressing the doped powder to compact pellets. With the quantification approach worked out and described here accurate analysis results with small uncertainties can be achieved for most elements of periodic table in almost every matrix composition. Furthermore direct traceability of the analytical results to the International System of Units (SI) is provided ensuring their higher metrological quality. Numerous additional systematic investigations concerning the preparation of the synthetic standards and their properties were carried out. The results of calibration of GD-MS instruments with synthetic standards for Co (Co-C), Cu, In, Fe and Zn matrices were checked by measuring CRMs. These results were also contrasted with those of other quantification approaches, as usually used in GD-MS routine. The results achieved with synthetic standards had the highest accuracy. The successful participation in the round robin test CCQM-P107 between international

Homogeneity study on biological candidate reference materials: the role of neutron activation analysis

Energy Technology Data Exchange (ETDEWEB)

Silva, Daniel P.; Moreira, Edson G., E-mail: dsilva.pereira@usp.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

2015-07-01

Instrumental Neutron activation Analysis (INAA) is a mature nuclear analytical technique able to accurately determine chemical elements without the need of sample digestion and, hence, without the associated problems of analyte loss or contamination. This feature, along with its potentiality use as a primary method of analysis, makes it an important tool for the characterization of new references materials and in the assessment of their homogeneity status. In this study, the ability of the comparative method of INAA for the within-bottle homogeneity of K, Mg, Mn and V in a mussel reference material was investigated. Method parameters, such as irradiation time, sample decay time and distance from sample to the detector were varied in order to allow element determination in subsamples of different sample masses in duplicate. Sample masses were in the range of 1 to 250 mg and the limitations of the detection limit for small sample masses and dead time distortions for large sample masses were investigated. (author)

The NIST natural-matrix radionuclide standard reference material program for ocean studies

International Nuclear Information System (INIS)

Inn, K.G.W.; Zhichao Lin; Zhongyu Wu; MacMahon, C.; Filliben, J.J.; Krey, P.; Feiner, M.; Harvey, J.

2001-01-01

In 1997, the Low-level Working Group of the International Committee on Radionuclide Metrology met in Boston, MA (USA) to define the characteristics of a new set of environmental radioactivity reference materials. These reference materials were to provide the radiochemist with the same analytical challenges faced when assaying environmental samples. It was decided that radionuclide bearing natural materials should be collected from sites where there had been sufficient time for natural processes to redistribute the various chemically different species of the radionuclides. Over the succeeding years, the National Institute of Standards and Technology (NIST), in cooperation with other highly experienced laboratories, certified and issued a number of these as low-level radioactivity Standard Reference Materials (SRMs) for fission and activation product and actinide concentrations. The experience of certifying these SRMs has given NIST the opportunity to compare radioanalytical methods and learn of their limitations. NIST convened an international workshop in 1994 to define the natural-matrix radionuclide SRM needs for ocean studies. The highest priorities proposed at the workshop were for sediment, shellfish, seaweed, fish flesh and water matrix SRMs certified for mBq per sample concentrations of 90 Sr, 137 Cs and 239 Pu + 240 Pu. The most recent low-level environmental radionuclide SRM issued by NIST, Ocean Sediment (SRM 4357) has certified and uncertified values for the following 22 radionuclides: 40 K, 90 Sr, 129 I, 137 Cs, 155 Eu, 210 Pb, 210 Po, 212 Pb, 214 Bi, 226 Ra, 228 Ra, 228 Th, 230 Th, 232 Th, 234 U, 235 U, 237 Np, 238 U, 238 Pu, 239 Pu + 240 Pu, and 241 Am. The uncertainties for a number of the certified radionuclides are non-symmetrical and relatively large because of the non-normal distribution of reported values. NIST is continuing its efforts to provide the ocean studies community with additional natural matrix radionuclide SRMs. The freeze

DEVELOPMENT OF THE REFERENCE MATERIALS PRODUCTION BRANCH IN THE JOINT STOCK COMPANY "THE GULIDOV KRASNOYARSK NON-FERROUS METALS PLANT"

Directory of Open Access Journals (Sweden)

K. A. Shatnykh

2015-01-01

Full Text Available The article deals with the development of the branch for the reference materials production in the Joint Stock Company "The Gulidov Krasnoyarsk Non-Ferrous Metals Plant" (JSC "Krastsvetmet". Here the most important workings for reference materials including the work for the London precious metal exchange, current and future works are stated.

Reference Material Kydex(registered trademark)-100 Test Data Message for Flammability Testing

Science.gov (United States)

Engel, Carl D.; Richardson, Erin; Davis, Eddie

2003-01-01

The Marshall Space Flight Center (MSFC) Materials and Processes Technical Information System (MAPTIS) database contains, as an engineering resource, a large amount of material test data carefully obtained and recorded over a number of years. Flammability test data obtained using Test 1 of NASA-STD-6001 is a significant component of this database. NASA-STD-6001 recommends that Kydex 100 be used as a reference material for testing certification and for comparison between test facilities in the round-robin certification testing that occurs every 2 years. As a result of these regular activities, a large volume of test data is recorded within the MAPTIS database. The activity described in this technical report was undertaken to mine the database, recover flammability (Test 1) Kydex 100 data, and review the lessons learned from analysis of these data.

Effect of reference parameters and properties of materials for WWER-type fuel elements on their reliability

Energy Technology Data Exchange (ETDEWEB)

Bibilashvili, Yu K; Malachenko, L L; Medvedev, A V; Solyany, V I; Sukhanov, G I; Tonkov, V Yu

1987-05-01

Present approach to requirements for reference parameters and properties of materials for WWER-1000 fuel elements is presented as well as evaluation of their effects on fuel reliability. Some results of investigations with the aim of improving fuel element reliability in operational NPP conditions are discussed. 4 references, 7 figures, 3 tables.

Japanese tea leaves: a possible biological standard reference material

International Nuclear Information System (INIS)

Fuwa, Keiichiro; Notsu, Kenji; Tsunoda, Kin-ichi; Kato, Hideaki; Yamamoto, Yuko.

1978-01-01

Japanese Tea Leaves, prepared by pulverizing with an agate ball mill and sieving with a Saran fiber sieve (50 mesh) were assessed as a possible biological standard reference material for elemental analysis. The metal content of the tea leaves was determined independently at two laboratories using atomic absorption and flame emission spectrometry. Neutron activation analysis was also performed to determine the content (21 elements) of Tea Leaves. For some elements the result from the various methods were compared. The characteristics of Tea Leaves are discussed and the elemental composition is compared to that of Orchard Leaves (NBS SRM, 1571). The most significant characteristic of Tea Leaves was the high manganese content. (auth.)

Certification of a niobium metal reference material for neutron dosimetry (EC-NRM 525)

International Nuclear Information System (INIS)

Lievens, F.; Ingelbrecht, C.; Pauwels, J.

1990-01-01

Niobium metal, of 99.98% nominal purity, in the form of 0.02 and 0.1 mm thick foils and of 0.5 mm diameter wire, has been certified for its tantalum mass fraction. The certified value of the tantalum mass fraction is 19.6 ± 1.8 mg.kg -1 and is based on 71 results obtained by six laboratories by neutron activation analysis or inductively coupled plasma source mass spectrometry. The material is intended to be used as a reference material in neutron metrology

Multivariate methods for analysis of environmental reference materials using laser-induced breakdown spectroscopy

Directory of Open Access Journals (Sweden)

Shikha Awasthi

2017-06-01

Full Text Available Analysis of emission from laser-induced plasma has a unique capability for quantifying the major and minor elements present in any type of samples under optimal analysis conditions. Chemometric techniques are very effective and reliable tools for quantification of multiple components in complex matrices. The feasibility of laser-induced breakdown spectroscopy (LIBS in combination with multivariate analysis was investigated for the analysis of environmental reference materials (RMs. In the present work, different (Certified/Standard Reference Materials of soil and plant origin were analyzed using LIBS and the presence of Al, Ca, Mg, Fe, K, Mn and Si were identified in the LIBS spectra of these materials. Multivariate statistical methods (Partial Least Square Regression and Partial Least Square Discriminant Analysis were employed for quantitative analysis of the constituent elements using the LIBS spectral data. Calibration models were used to predict the concentrations of the different elements of test samples and subsequently, the concentrations were compared with certified concentrations to check the authenticity of models. The non-destructive analytical method namely Instrumental Neutron Activation Analysis (INAA using high flux reactor neutrons and high resolution gamma-ray spectrometry was also used for intercomparison of results of two RMs by LIBS.

Production of Working Reference Materials for the Capability Evaluation Project

Energy Technology Data Exchange (ETDEWEB)

Phillip D. Noll, Jr.; Robert S. Marshall

1999-03-01

Nondestructive waste assay (NDA) methods are employed to determine the mass and activity of waste-entrained radionuclides as part of the National TRU (Trans-Uranic) Waste Characterization Program. In support of this program the Idaho National Engineering and Environmental Laboratory Mixed Waste Focus Area developed a plan to acquire capability/performance data on systems proposed for NDA purposes. The Capability Evaluation Project (CEP) was designed to evaluate the NDA systems of commercial contractors by subjecting all participants to identical tests involving 55 gallon drum surrogates containing known quantities and distributions of radioactive materials in the form of sealed-source standards, referred to as working reference materials (WRMs). Although numerous Pu WRMs already exist, the CEP WRM set allows for the evaluation of the capability and performance of systems with respect to waste types/configurations which contain increased amounts of {sup 241}Am relative to weapons grade Pu, waste that is dominantly {sup 241}Am, as well as wastes containing various proportions of depleted uranium. The CEP WRMs consist of a special mixture of PuO{sub 2}/AmO{sub 2} (IAP) and diatomaceous earth (DE) or depleted uranium (DU) oxide and DE and were fabricated at Los Alamos National Laboratory. The IAP WRMS are contained inside a pair of welded inner and outer stainless steel containers. The DU WRMs are singly contained within a stainless steel container equivalent to the outer container of the IAP standards. This report gives a general overview and discussion relating to the production and certification of the CEP WRMs.

Electrodynamics in Arbitrary Reference Frames and in Arbitrary Material Media

International Nuclear Information System (INIS)

Horzela, A.; Kapuscik, E.; Widomski, M.

1999-01-01

Full text: The investigation of electromagnetic phenomena in material media still belongs to the most difficult tasks of electrodynamics. Complexity and variability of material media practically exclude effective applications of methods and computational techniques elaborated in the framework of standard microscopic electrodynamics with classical vacuum as a ground state. In order to obtain satisfactorily exact descriptions of electromagnetic properties of complex material media one is enforced to use methods and approximations which are difficult to control. Moreover, they usually break covariance properties and the results obtained are valid in one reference frame which choice remains subjective and model dependent. Some time ago we have proposed a reformulation of Maxwell electrodynamics which opens new ways in study of electromagnetic processes in material media. The formalism gets rid of assumptions characteristic for vacuum electrodynamics only and it avoids the usage of constitutive relations as primary relations put on quantities needed for a complete description of an electromagnetic system. Fundamental properties of all electromagnetic quantities are their uniquely defined transformation rules and their analysis allows to determine the possible relations between them. Within such a scheme it is possible to introduce constitutive relations which do not have analogies in macroscopic classical electrodynamics. They may be used in description of microscopic electromagnetic processes in a different way than it is done in the framework of quantum electrodynamics. (author)

Production of NDA Working Reference Materials for the Capability Evaluation Project

International Nuclear Information System (INIS)

Noll, P.D. Jr.; Marshall, R.S.

1998-01-01

The production of Non Destructive Assay (NDA) Working Reference Materials (WRMs) that are traceable to nationally recognized standards was undertaken to support implementation of the Idaho National Engineering and Environmental Laboratory (INEEL) Nondestructive Waste Assay Capability Evaluation Project (CEP). The WRMs produced for the CEP project consist of Increased Am/Pu mass ration (IAP) and depleted Uranium (DU) WRMs. The CEP IAP/DU WRM set provides radioactive material standards for use in combination with 55 gallon drum waste matrix surrogates for the assessment of waste NDA assay system performance. The Production of WRMs is a meticulous process that is not without certain trials and tribulations. Problems may arise at any of the various stages of WRM production which include, but are not limited to; material characterization (physical, chemical, and isotopic), material blend parameters, personnel radiation exposure, gas generation phenomenon, traceability to national standards, encapsulation, statistical evaluation of the data, and others. Presented here is an overall description of the process by which the CEP WRMs were produced and certified as well as discussions pertaining to some of the problems encountered and how they were solved

IAEA reference materials for quality assurance of marine radioactivity measurements

International Nuclear Information System (INIS)

Povinec, P.P.; Pham, M.K.

2001-01-01

The IAEA's Marine Environment Laboratory has been assisting laboratories in Analytical Quality Control Services (AQCS) for the analysis of radionuclides in the marine environment since the early seventies. AQCS through world-wide and regional intercomparison exercises and the provision of reference methods and reference materials (RM) have been recognized as an important component of quality assurance/quality control. A total of 43 intercomparison exercises were organized and 37 RM were produced for marine radioactivity studies. All important marine matrices were covered, e.g., seawater, marine sediments of different chemical compositions, fish, shellfish and seaplants. RM were prepared from samples collected at contaminated sites (e.g., the Irish Sea, the Baltic Sea, the Arabian Sea, Mururoa and Bikini Atolls, etc.) as well as from sites affected only by global fallout (e.g., the Pacific Ocean). Available RM are listed in the IAEA biennial catalogue and can be purchased at a minimal price. An overview of prepared RM for radionuclides in marine matrices is presented and discussed in more detail. (author)

Reference materials and interlaboratory comparison for actinide analysis

International Nuclear Information System (INIS)

Hanssens, Alain; Viallesoubranne, Carole; Roche, Claude; Liozon, Gerard

2008-01-01

Measurement quality is crucial for the safety of nuclear facilities and is a primary requirement for fissile material monitoring and accountancy. CETAMA (Cea Committee for the establishment of analysis methods), in collaboration with Cea and AREVA laboratories, fabricates certified reference materials and organizes interlaboratory comparison programs for plutonium and uranium assay in solution. A new plutonium metal measurement standard (MP3) is currently being prepared by Cea and is a subject of cooperative work in view of its certification and use by analysis laboratories. U and Pu interlaboratory comparisons are carried out at regular intervals on benchmark samples in coordination with working groups from French nuclear laboratories. These programs are supported by international cooperation. 'Chemical' methods (potentiometry, gravimetric analysis, etc.) generally provide the best accuracy. Coulometry is the benchmark technique for plutonium assay: its metrological qualities should be an incentive for wider use by laboratories performing precise control assays of plutonium as well as uranium. Gravimetric analysis provides excellent results for analysis of pure uranyl nitrate solutions. In view of its many advantages we encourage laboratories to employ this technique to assay pure U or Pu solutions. 'Physical' or 'physicochemical' methods are increasingly used, and their performance has improved. K-edge absorption spectrometry and isotope dilution mass spectrometry are capable of reaching measurement quality levels comparable to those of the best 'chemical' methods. (authors)

The role of adequate reference materials in density measurements in hemodialysis

Science.gov (United States)

Furtado, A.; Moutinho, J.; Moura, S.; Oliveira, F.; Filipe, E.

2015-02-01

In hemodialysis, oscillation-type density meters are used to measure the density of the acid component of the dialysate solutions used in the treatment of kidney patients. An incorrect density determination of this solution used in hemodialysis treatments can cause several and adverse events to patients. Therefore, despite the Fresenius Medical Care (FME) tight control of the density meters calibration results, this study shows the benefits of mimic the matrix usually measured to produce suitable reference materials for the density meter calibrations.

The role of adequate reference materials in density measurements in hemodialysis

International Nuclear Information System (INIS)

Furtado, A; Moura, S; Filipe, E; Moutinho, J; Oliveira, F

2015-01-01

In hemodialysis, oscillation-type density meters are used to measure the density of the acid component of the dialysate solutions used in the treatment of kidney patients. An incorrect density determination of this solution used in hemodialysis treatments can cause several and adverse events to patients. Therefore, despite the Fresenius Medical Care (FME) tight control of the density meters calibration results, this study shows the benefits of mimic the matrix usually measured to produce suitable reference materials for the density meter calibrations

Development of benzene, toluene, ethylbenzene and xylenes certified gaseous reference materials

Science.gov (United States)

Brum, M. C.; Sobrinho, D. C. G.; Fagundes, F. A.; Oudwater, R. J.; Augusto, C. R.

2016-07-01

The work describes the production of certified gaseous reference materials of benzene, toluene, ethylbenzene and xylenes (BTEX) in nitrogen from the gravimetric production up to the long term stability tests followed by the certifying step. The uncertainty in the amount fractions of the compounds in these mixtures was approximately 4% (relative) for the range studied from 2 to 16 µmol/mol. Also the adsorption of the BTEX on the cylinder surface and the tubing were investigated as potential uncertainty source.

Use of reference materials for quality control of elemental analysis by neutron activation with radiochemical separation

International Nuclear Information System (INIS)

Woittiez, J.R.W.

1990-01-01

This paper describes the use of certified reference materials to monitor the long-term quality of radiochemical separations. The practical limitations which determine the actual design of the quality control are discussed. The hypothesis that the high yield of the radiochemical separation will be constant with time has been checked and validated for the elements Zn, Fe, Co, Cd, Mo and to a lesser extent for W and Th using NBS SRM 1577A, BCR CRM 274 and IAEA RM A-11. This validation could not be made for the elements Cr, Au, and Ag. Especially for Cr there is a serious lack of appropiate certified reference materials. (orig.)

Nicotine, acetanilide and urea multi-level2H-,13C- and15N-abundance reference materials for continuous-flow isotope ratio mass spectrometry

Science.gov (United States)

Schimmelmann, A.; Albertino, A.; Sauer, P.E.; Qi, H.; Molinie, R.; Mesnard, F.

2009-01-01

Accurate determinations of stable isotope ratios require a calibration using at least two reference materials with different isotopic compositions to anchor the isotopic scale and compensate for differences in machine slope. Ideally, the S values of these reference materials should bracket the isotopic range of samples with unknown S values. While the practice of analyzing two isotopically distinct reference materials is common for water (VSMOW-SLAP) and carbonates (NBS 19 and L-SVEC), the lack of widely available organic reference materials with distinct isotopic composition has hindered the practice when analyzing organic materials by elemental analysis/isotope ratio mass spectrometry (EA-IRMS). At present only L-glutamic acids USGS40 and USGS41 satisfy these requirements for ??13C and ??13N, with the limitation that L-glutamic acid is not suitable for analysis by gas chromatography (GC). We describe the development and quality testing of (i) four nicotine laboratory reference materials for on-line (i.e. continuous flow) hydrogen reductive gas chromatography-isotope ratio mass-spectrometry (GC-IRMS), (ii) five nicotines for oxidative C, N gas chromatography-combustion-isotope ratio mass-spectrometry (GC-C-IRMS, or GC-IRMS), and (iii) also three acetanilide and three urea reference materials for on-line oxidative EA-IRMS for C and N. Isotopic off-line calibration against international stable isotope measurement standards at Indiana University adhered to the 'principle of identical treatment'. The new reference materials cover the following isotopic ranges: ??2Hnicotine -162 to -45%o, ??13Cnicotine -30.05 to +7.72%, ?? 15Nnicotine -6.03 to +33.62%; ??15N acetanilide +1-18 to +40.57%; ??13Curea -34.13 to +11.71%, ??15Nurea +0.26 to +40.61% (recommended ?? values refer to calibration with NBS 19, L-SVEC, IAEA-N-1, and IAEA-N-2). Nicotines fill a gap as the first organic nitrogen stable isotope reference materials for GC-IRMS that are available with different ??13N

Feasibility of the development of reference materials for the detection of Ag nanoparticles in food: neat dispersions and spiked chicken meat

NARCIS (Netherlands)

Grombe, R.; Allmaier, G.; Charoud-Got, J.; Dudkiewicz, A.; Emteborg, H.; Hofmann, T.; Huusfeldt-Larsen, E.; Lehner, A.; Llinas, M.; Loeschner, K.; Molhave, K.; Peters, R.J.B.; Seghers, J.; Solans, C.; Kammer, van den F.; Wagner, S.; Weigel, S.; Linsinger, T.P.J.

2015-01-01

The feasibility of producing colloidal silver nanoparticle reference materials and silver nanoparticle spiked reference matrix materials was investigated. Two concentrations of PVP-coated silver nanoparticle dispersions were evaluated and used to spike chicken meat, with the aim of producing a set

On the system of provision of ojsc "MMC 'Norilsk Nickel'" with interstate and State certified reference materials for quality control of cobalt, nickel, copper and promproducts

Directory of Open Access Journals (Sweden)

T. V. Shabelnikova

2014-01-01

Full Text Available In order to manage the quality of OJSC "MMC "Norilsk Nickel" products the Centre of Certified Reference Material Development has developed and is currently successfully implementing a system of operations provision with interstate and state certified reference materials of nickel, cobalt and copper composition. The system wholly corresponds to modern metrological requirements. The Centre of Reference Materials Development, fulfilling leading function in the field of state certified reference material production and supply to the Company's operations, aims its activity both at the development of new types of certified reference materials in the form of metals and at widening the range of synthetic oxide certified reference materials. Developed for the first time, metallic state certified reference materials of nickel, cobalt composition with certified mass fractions of oxygen, hydrogen, nitrogen, sulfur and carbon were put into practice of the Company's analytical services work. Certified reference material use provides the possibility to take into account requirements of some consumers to the quality of nickel and produce by OJSC "MMC "Norilsk Nickel" and also helps to raise competitive ability of the products on the world metals market. Over recent years the Centre fulfilled the work on the development, certification in established order, approval and entering into the State Register twenty five types of state certified reference materials. Certified reference materials are intended for fulfillment of the analysis of chemical composition of nickel, cobalt and copper in terms of their conformity with both national and international standards.

The preparation and certification of a South African phosphate concentrate for use as a reference material

International Nuclear Information System (INIS)

Hansen, R.G.

1985-01-01

This report describes the preparation, analysis, and certification of South African Reference Material (SARM) 32. The material is a phosphate concentrate from the Phalaborwa deposit, and was supplied by the Phosphate Development Corporation Ltd (Foskor). Eighteen laboratories in eight countries used a variety of analytical techniques to provide the analytical results

Iodine in different food articles and standard reference materials

International Nuclear Information System (INIS)

Dermelj, M.; Slejkovec, Z.; Byrne, A.R.; Stegnar, P.; Stibilj, V.; Rossbach, M.

1990-01-01

The greater part of essential iodine enters living organisms via the food chain. Nevertheless, quantitative data on its concentration in diets, food articles and also in available SRMs are very poor and scarce. This and WHO recommendations on daily allowances of iodine for man via food articles caused an added demand for accurate and reliable determination of iodine in these samples. From this point of view the purpose of the present was to analyse and to establish the concentration levels of total iodine in some food articles, diets, SRMs and candidate reference materials by the use of rapid radiochemical separation, developed in our laboratory. The results were checked by the analysis of SRMs with available certified values for iodine and good agreement is evident. (orig.)

Bias detection and certified reference materials for random measurands

Science.gov (United States)

Rukhin, Andrew L.

2015-12-01

A problem that frequently occurs in metrology is the bias checking of data obtained by a laboratory against the specified value and uncertainty estimate given in the certificate of analysis. The measurand—a property of a certified reference material (CRM)—is supposed to be random with a normal distribution whose parameters are given by the certificate specifications. The laboratory’s data from subsequent measurements of the CRM (a CRM experiment) are summarized by the sample mean value and its uncertainty which is commonly based on a repeatability standard deviation. New confidence intervals for the lab’s bias are derived. Although they may lack intuitive appeal, those obtained by using higher order asymptotic methods, compared and contrasted in this paper, are recommended.

The application of the k0-standardization method at the TRIGA Mark II reactor, Ljubljana, Slovenia

International Nuclear Information System (INIS)

Jacimovic, Radojko; Benedik, Ljudmila; Stegnar, Peter; Smodis, Borut

2002-01-01

The k 0 -standardization method of neutron activation analysis (k 0 -NAA) was launched in the 1970s and since then continuously developed. Nowadays, k 0 -NAA became widespread as a practical analytical tool used to analyse different sample matrices. At the Jozef Stefan Institute (IJS), the KAYZERO/SOLCOI software package has been introduced for data processing after extensive testing and comparison with other available programs. In the process of validation of the software a suite of natural matrix reference materials (RMs) were used. Five certified reference materials (CRMs) from the Institute for Reference Materials and Measurements (IRMM), two standard reference materials (SRMs) from the National Institute of Standards and Technology (NIST), three RMs from the International Atomic Energy Agency (IAEA) and one RM from IJS were analysed. Altogether, results for ten elements in inorganic matrices and twenty-one elements in organic matrices, obtained by k 0 -instrumental neutron activation analysis (k 0 -INAA), were compared to certified values. The results obtained show good agreement with certified or assigned values except for Fe and U in inorganic matrices, and Al and Cr in organic matrices. (author)

Preparation of an In-House Reference Material Containing Fumonisins in Thai Rice and Matrix Extension of the Analytical Method for Japanese Rice

Science.gov (United States)

Awaludin, Norhafniza; Nagata, Reiko; Kawasaki, Tomomi; Kushiro, Masayo

2009-01-01

Mycotoxin contamination in rice is less reported, compared to that in wheat or maize, however, some Fusarium fungi occasionally infect rice in the paddy field. Fumonisins are mycotoxins mainly produced by Fusarium verticillioides, which often ruins maize. Rice adherent fungus Gibberella fujikuroi is taxonomically near to F. verticillioides, and there are sporadic reports of fumonisin contamination in rice from Asia, Europe and the United States. Therefore, there exists the potential risk of fumonisin contamination in rice as well as the need for the validated analytical method for fumonisins in rice. Although both natural and spiked reference materials are available for some Fusarium mycotoxins in matrices of wheat and maize, there are no reference materials for Fusarium mycotoxins in rice. In this study, we have developed a method for the preparation of a reference material containing fumonisins in Thai rice. A ShakeMaster grinding machine was used for the preparation of a mixed material of blank Thai rice and F. verticillioides-infected Thai rice. The homogeneity of the mixed material was confirmed by one-way analysis of variance, which led this material to serve as an in-house reference material. Using this reference material, several procedures to extract fumonisins from Thai rice were compared. Accordingly, we proved the applicability of an effective extraction procedure for the determination of fumonisins in Japanese rice. PMID:22069540

Preparation and certification of the Polish reference material 'Oriental Tobacco Leaves' (CTA-OTL-1) for inorganic trace analysis

International Nuclear Information System (INIS)

Dybczynski, R.; Polkowska-Motrenko, H.; Samczynski, Z.; Szopa, Z.

1996-01-01

A new Polish certified reference material 'Oriental Tobacco Leaves' (CTA-OTL-1) for inorganic trace analysis was prepared. Fresh tobacco leaves of variety 'Oriental' were dried, ground and sieved. All precautions were taken to avoid contamination of material with metals. The next step was homogenization. Preliminary homogeneity checking consisted in determining of Ca, Fe and K content by X-ray fluorescence. Final homogeneity testing was performed by neutron activation analysis determining Co, Cr, Fe and Rb. To assure long-term stability, the whole lot of material was sterilized by electron beam radiation. Certification of the candidate reference material was done on the basis of world-wide interlaboratory comparisons exercise in which 61 laboratories, using various analytical methods participated. (author). 30 refs, 12 tabs, 21 figs

Preparation and certification of the Polish reference material `Oriental Tobacco Leaves` (CTA-OTL-1) for inorganic trace analysis

Energy Technology Data Exchange (ETDEWEB)

Dybczynski, R.; Polkowska-Motrenko, H.; Samczynski, Z.; Szopa, Z. [Institute of Nuclear Chemistry and Technology, Warsaw (Poland)

1996-12-31

A new Polish certified reference material `Oriental Tobacco Leaves` (CTA-OTL-1) for inorganic trace analysis was prepared. Fresh tobacco leaves of variety `Oriental` were dried, ground and sieved. All precautions were taken to avoid contamination of material with metals. The next step was homogenization. Preliminary homogeneity checking consisted in determining of Ca, Fe and K content by X-ray fluorescence. Final homogeneity testing was performed by neutron activation analysis determining Co, Cr, Fe and Rb. To assure long-term stability, the whole lot of material was sterilized by electron beam radiation. Certification of the candidate reference material was done on the basis of world-wide interlaboratory comparisons exercise in which 61 laboratories, using various analytical methods participated. (author). 30 refs, 12 tabs, 21 figs.

Phosphated minerals to be used as radioactive reference materials; Minerais fosfatados para serem utilizados como materiais de referencia radioativos

Energy Technology Data Exchange (ETDEWEB)

Braganca, M.J.C.S.; Tauhata, L. [Instituto de Radioprotecao e Dosimetria (IRD/CNEN-RJ), Rio de Janeiro, RJ (Brazil). Lab. Nacional de Metrologia das Radiacoes Ionizantes (LNMRI); Clain, A.F. [Universidade Severino Sombra, Vassouras, RJ (Brazil); Moreira, I. [Pontificia Univ. Catolica do Rio de Janeiro (PUC/Rio), RJ (Brazil). Dept. de Quimica

2003-07-01

The production and the supplying of certified reference materials, or deliberated contaminated materials containing natural radionuclides for laboratories which analyses environmental samples are fundamentals for the correct measurements of their radioactive levels. This analysis quality represents a important step for the safeguards of the population health, and quality control of the imported and exported products, such as minerals, agricultural and raw materials. The phosphate rocks, containing significant concentrations of thorium, and used as raw material and fertilizers justified a study for better characterization and distinction to be used cas certified reference radioactive materials. Therefore, samples from the two carboanalytical-alkaline chimneys (Araxa and Catalao), and one from metasedimentar origin (Patos de Minas), distant 100 km from each other, were collected and chemical and cholecystographic characterized by optical emission, X-ray diffraction and fluorescence. The element concentrations were determined by neutron activation analysis, ICP-MS and ICP-AES. The results, after multivariate statistical analysis and study of correlations among elements, have shown geochemical similarities of the phosphates from Araxa and Catalao, and differences from Patos de Minas, despite of the geographic proximity. The concentration of thorium between 200 and 500 (mg/g) allows to use such minerals as reference materials.

Results of a Saxitoxin Proficiency Test Including Characterization of Reference Material and Stability Studies

Directory of Open Access Journals (Sweden)

Kirsi Harju

2015-11-01

Full Text Available A saxitoxin (STX proficiency test (PT was organized as part of the Establishment of Quality Assurance for the Detection of Biological Toxins of Potential Bioterrorism Risk (EQuATox project. The aim of this PT was to provide an evaluation of existing methods and the European laboratories’ capabilities for the analysis of STX and some of its analogues in real samples. Homogenized mussel material and algal cell materials containing paralytic shellfish poisoning (PSP toxins were produced as reference sample matrices. The reference material was characterized using various analytical methods. Acidified algal extract samples at two concentration levels were prepared from a bulk culture of PSP toxins producing dinoflagellate Alexandrium ostenfeldii. The homogeneity and stability of the prepared PT samples were studied and found to be fit-for-purpose. Thereafter, eight STX PT samples were sent to ten participating laboratories from eight countries. The PT offered the participating laboratories the possibility to assess their performance regarding the qualitative and quantitative detection of PSP toxins. Various techniques such as official Association of Official Analytical Chemists (AOAC methods, immunoassays, and liquid chromatography-mass spectrometry were used for sample analyses.

Determination of trace elements in the human hair reference material, HH-I, by neutron activation analysis and atomic absorption spectrophotometry

International Nuclear Information System (INIS)

Coetzee, P.; Pieterse, H.

1986-01-01

Analytical procedures are presented and problem areas identified with regard to the determination of trace elements in IAEA powdered human hair reference material, HH-I, of limited sample size (100-200 mg), by NAA and graphite furnace AAS. Results obtained for the twelve elements As, Cd, Co, Cr, Cu, Fe, Hg, Mn, Ni, Sb, Se, and Zn studied in human hair and other biological reference material like orchard leaves, seaplant material, and copepod compare satisfactorily with the certified values

Grain-size effects on PIXE and INAA analysis of IAEA-336 lichen reference material

International Nuclear Information System (INIS)

Marques, A.P.; Freitas, M.C.; Wolterbeek, H.Th.; Verburg, T.G.; Goeij, J.J.M. de

2007-01-01

IAEA-336 lichen certified reference material was used to compare outcomes from INAA and PIXE elemental analyses, in relationship with grain size. The IAEA material (grain size <125 μm) was ground and sieved through nylon nets with 64 μm, 41 μm and 20 μm pores. Particle sizes were determined by Laser Light Scattering technique: the data indicate that, after sieving, the IAEA-336 lichen reference material's particle size distribution follows a bimodal distribution, which is turning more and more monomodal after further fine sieving. Replicates of each fraction were analysed by INAA and PIXE. Results for Cl, K, Mn, Fe and Zn by both techniques were compared by application of z-values tested against the criterion vertical bar z vertical bar < 3 for approval of results at the 99.7% confidence level. Under the conditions of this study, the limited amount of lichen material as 'seen' in the PIXE analysis and the grain size distribution in the lichen material were no causes of measurable differences between the results of both techniques. However, fractionation into smaller grain sizes showed to be associated with lower element content, for Na, Cl, K, Mn and Sr even up to a factor of 2. The observed increases of the proportion of algae in the smaller grain-size fractions and the possible accumulation capacity for certain elements in the fungal part of the lichen may explain the observed phenomenon. The sieving process and consequently the discarding of part of the material have lead to a change of the properties of the original sample, namely algae/fungus percentage and elemental contents

Determination of trimethyllead reference material using high performance liquid chromatography-inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Lu Hai; Wei Chao; Wang Jun; Chao Jingbo; Zhou Tao; Chen Dazhou

2005-01-01

A high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICPMS) was combined, and the chromatography conditions were optimized. The stability and homogeneity of a trimethyllead reference material were determined using this method. (authors)

Scalar material reference systems and loop quantum gravity

International Nuclear Information System (INIS)

Giesel, K; Thiemann, T

2015-01-01

In the past, the possibility to employ (scalar) material reference systems in order to describe classical and quantum gravity directly in terms of gauge invariant (Dirac) observables has been emphasized frequently. This idea has been picked up more recently in loop quantum gravity with the aim to perform a reduced phase space quantization of the theory, thus possibly avoiding problems with the (Dirac) operator constraint quantization method for a constrained system. In this work, we review the models that have been studied on the classical and/or the quantum level and parametrize the space of theories considered so far. We then describe the quantum theory of a model that, to the best of our knowledge, has only been considered classically so far. This model could arguably be called the optimal one in this class of models considered as it displays the simplest possible true Hamiltonian, while at the same time reducing all constraints of general relativity. (paper)

New Carbonate Standard Reference Materials for Boron Isotope Geochemistry

Science.gov (United States)

Stewart, J.; Christopher, S. J.; Day, R. D.

2015-12-01

The isotopic composition of boron (δ11B) in marine carbonates is well established as a proxy for past ocean pH. Yet, before palaeoceanographic interpretation can be made, rigorous assessment of analytical uncertainty of δ11B data is required; particularly in light of recent interlaboratory comparison studies that reported significant measurement disagreement between laboratories [1]. Well characterised boron standard reference materials (SRMs) in a carbonate matrix are needed to assess the accuracy and precision of carbonate δ11B measurements throughout the entire procedural chemistry; from sample cleaning, to ionic separation of boron from the carbonate matrix, and final δ11B measurement by multi-collector inductively coupled plasma mass spectrometry. To date only two carbonate reference materials exist that have been value-assigned by the boron isotope measurement community [2]; JCp-1 (porites coral) and JCt-1 (Giant Clam) [3]. The National Institute of Standards and Technology (NIST) will supplement these existing standards with new solution based inorganic carbonate boron SRMs that replicate typical foraminiferal and coral B/Ca ratios and δ11B values. These new SRMs will not only ensure quality control of full procedural chemistry between laboratories, but have the added benefits of being both in abundant supply and free from any restrictions associated with shipment of biogenic samples derived from protected species. Here we present in-house δ11B measurements of these new boron carbonate SRM solutions. These preliminary data will feed into an interlaboratory comparison study to establish certified values for these new NIST SRMs. 1. Foster, G.L., et al., Chemical Geology, 2013. 358(0): p. 1-14. 2. Gutjahr, M., et al., Boron Isotope Intercomparison Project (BIIP): Development of a new carbonate standard for stable isotopic analyses. Geophysical Research Abstracts, EGU General Assembly 2014, 2014. 16(EGU2014-5028-1). 3. Inoue, M., et al., Geostandards and

Current mass spectrometry strategies for selenium speciation in dietary sources of high-selenium

Energy Technology Data Exchange (ETDEWEB)

Infante, Heidi Goenaga; Hearn, Ruth; Catterick, Tim [LGC Limited, Teddington, Middlesex (United Kingdom)

2005-06-01

This document reviews the most relevant mass spectrometry approaches to selenium (Se) speciation in high-Se food supplements in terms of qualitative and quantitative Se speciation and Se-containing species identification, with special reference to high-Se yeast, garlic, onions and Brazil nuts. Important topics such as complexity of Se speciation in these materials and the importance of combining Se-specific detection and molecule-specific determination of the particular species of this element in parallel with chromatography, to understand their nutritional role and cancer preventive properties are critically discussed throughout. The versatility and potential of mass spectrometric detection in this field are clearly demonstrated. Although great advances have been achieved, further developments are required, especially if ''speciated''certified reference materials (CRMs) are to be produced for validation of measurements of target Se-containing species in Se-food supplements. (orig.)

Nicotine, acetanilide and urea multi-level 2H-, 13C- and 15N-abundance reference materials for continuous-flow isotope ratio mass spectrometry.

Science.gov (United States)

Schimmelmann, Arndt; Albertino, Andrea; Sauer, Peter E; Qi, Haiping; Molinie, Roland; Mesnard, François

2009-11-01

Accurate determinations of stable isotope ratios require a calibration using at least two reference materials with different isotopic compositions to anchor the isotopic scale and compensate for differences in machine slope. Ideally, the delta values of these reference materials should bracket the isotopic range of samples with unknown delta values. While the practice of analyzing two isotopically distinct reference materials is common for water (VSMOW-SLAP) and carbonates (NBS 19 and L-SVEC), the lack of widely available organic reference materials with distinct isotopic composition has hindered the practice when analyzing organic materials by elemental analysis/isotope ratio mass spectrometry (EA-IRMS). At present only L-glutamic acids USGS40 and USGS41 satisfy these requirements for delta13C and delta15N, with the limitation that L-glutamic acid is not suitable for analysis by gas chromatography (GC). We describe the development and quality testing of (i) four nicotine laboratory reference materials for on-line (i.e. continuous flow) hydrogen reductive gas chromatography-isotope ratio mass-spectrometry (GC-IRMS), (ii) five nicotines for oxidative C, N gas chromatography-combustion-isotope ratio mass-spectrometry (GC-C-IRMS, or GC-IRMS), and (iii) also three acetanilide and three urea reference materials for on-line oxidative EA-IRMS for C and N. Isotopic off-line calibration against international stable isotope measurement standards at Indiana University adhered to the 'principle of identical treatment'. The new reference materials cover the following isotopic ranges: delta2H(nicotine) -162 to -45 per thousand, delta13C(nicotine) -30.05 to +7.72 per thousand, delta15N(nicotine) -6.03 to +33.62 per thousand; delta15N(acetanilide) +1.18 to +40.57 per thousand; delta13C(urea) -34.13 to +11.71 per thousand, delta15N(urea) +0.26 to +40.61 per thousand (recommended delta values refer to calibration with NBS 19, L-SVEC, IAEA-N-1, and IAEA-N-2). Nicotines fill a gap as

Reference materials and interlaboratory comparison for actinide analysis

Energy Technology Data Exchange (ETDEWEB)

Hanssens, Alain; Viallesoubranne, Carole; Roche, Claude; Liozon, Gerard [Commissariat a l' Energie Atomique, Marcoule: BP 17171, 30207 Bagnols sur Ceze (France)

2008-07-01

Measurement quality is crucial for the safety of nuclear facilities and is a primary requirement for fissile material monitoring and accountancy. CETAMA (Cea Committee for the establishment of analysis methods), in collaboration with Cea and AREVA laboratories, fabricates certified reference materials and organizes interlaboratory comparison programs for plutonium and uranium assay in solution. A new plutonium metal measurement standard (MP3) is currently being prepared by Cea and is a subject of cooperative work in view of its certification and use by analysis laboratories. U and Pu interlaboratory comparisons are carried out at regular intervals on benchmark samples in coordination with working groups from French nuclear laboratories. These programs are supported by international cooperation. 'Chemical' methods (potentiometry, gravimetric analysis, etc.) generally provide the best accuracy. Coulometry is the benchmark technique for plutonium assay: its metrological qualities should be an incentive for wider use by laboratories performing precise control assays of plutonium as well as uranium. Gravimetric analysis provides excellent results for analysis of pure uranyl nitrate solutions. In view of its many advantages we encourage laboratories to employ this technique to assay pure U or Pu solutions. 'Physical' or 'physicochemical' methods are increasingly used, and their performance has improved. K-edge absorption spectrometry and isotope dilution mass spectrometry are capable of reaching measurement quality levels comparable to those of the best 'chemical' methods. (authors)

The Kjeldahl method as a primary reference procedure for total protein in certified reference materials used in clinical chemistry. I. A review of Kjeldahl methods adopted by laboratory medicine.

Science.gov (United States)

Chromý, Vratislav; Vinklárková, Bára; Šprongl, Luděk; Bittová, Miroslava

2015-01-01

We found previously that albumin-calibrated total protein in certified reference materials causes unacceptable positive bias in analysis of human sera. The simplest way to cure this defect is the use of human-based serum/plasma standards calibrated by the Kjeldahl method. Such standards, commutative with serum samples, will compensate for bias caused by lipids and bilirubin in most human sera. To find a suitable primary reference procedure for total protein in reference materials, we reviewed Kjeldahl methods adopted by laboratory medicine. We found two methods recommended for total protein in human samples: an indirect analysis based on total Kjeldahl nitrogen corrected for its nonprotein nitrogen and a direct analysis made on isolated protein precipitates. The methods found will be assessed in a subsequent article.

Critical assessment of the performance of electronic moisture analyzers for small amounts of environmental samples and biological reference materials.

Science.gov (United States)

Krachler, M

2001-12-01

Two electronic moisture analyzers were critically evaluated with regard to their suitability for determining moisture in small amounts (environmental matrices such as leaves, needles, soil, peat, sediments, and sewage sludge, as well as various biological reference materials. To this end, several homogeneous bulk materials were prepared which were subsequently employed for the development and optimization of all analytical procedures. The key features of the moisture analyzers included a halogen or ceramic heater and an integrated balance with a resolution of 0.1 mg, which is an essential prerequisite for obtaining precise results. Oven drying of the bulk materials in a conventional oven at 105 degrees C until constant mass served as reference method. A heating temperature of 65degrees C was found to provide accurate and precise results for almost all matrices investigated. To further improve the accuracy and precision, other critical parameters such as handling of sample pans, standby temperature, and measurement delay were optimized. Because of its ponderous heating behavior, the performance of the ceramic radiator was inferior to that of the halogen heater, which produced moisture results comparable to those obtained by oven drying. The developed drying procedures were successfully applied to the fast moisture analysis (1.4-6.3 min) of certified biological reference materials of similar provenance to the investigated the bulk materials. Moisture results for 200 mg aliquots ranged from 1.4 to 7.8% and good agreement was obtained between the recommended drying procedure for the reference materials and the electronic moisture analyzers with absolute uncertainties amounting to 0.1% and 0.2-0.3%, respectively.

Uncertainty evaluation in normalization of isotope delta measurement results against international reference materials.

Science.gov (United States)

Meija, Juris; Chartrand, Michelle M G

2018-01-01

Isotope delta measurements are normalized against international reference standards. Although multi-point normalization is becoming a standard practice, the existing uncertainty evaluation practices are either undocumented or are incomplete. For multi-point normalization, we present errors-in-variables regression models for explicit accounting of the measurement uncertainty of the international standards along with the uncertainty that is attributed to their assigned values. This manuscript presents framework to account for the uncertainty that arises due to a small number of replicate measurements and discusses multi-laboratory data reduction while accounting for inevitable correlations between the laboratories due to the use of identical reference materials for calibration. Both frequentist and Bayesian methods of uncertainty analysis are discussed.

Reference Materials for Trace Element Microanalysis of Carbonates by SIMS and other Mass Spectrometric Techniques

Science.gov (United States)

Layne, G. D.

2009-12-01

Today, many areas of geochemical research utilize microanalytical determinations of trace elements in carbonate minerals. In particular, there has been an explosion in the application of Secondary Ion Mass Spectrometry (SIMS) to studies of marine biomineralization. SIMS provides highly precise determinations of Mg and Sr at the concentration levels normally encountered in corals, mollusks or fish otoliths. It is also a highly effective means for determining a wide range of other trace elements at ppm levels (e.g., Na, Fe, Mn, Ba, REE, Pb, Th, and U) in a variety of naturally occurring calcite and aragonite matrices - and so is potentially valuable in studies of diagenesis, hydrothermal fluids and carbonatitic magmas. For SIMS, modest time per spot (often sputtered ion yields of most elements with the major element composition of the sample matrix, accuracy of SIMS depends intimately on matrix-matched solid reference materials. Despite its rapidly increasing use for trace element analyses of carbonates, there remains a dearth of certified reference materials suitable for calibrating SIMS. The pressed powders used by some analysts to calibrate LA-ICP-MS do not perform well for SIMS - they are not perfectly dense or homogeneous to the desired level at the micron scale of sampling. Further, they often prove incompatible with the sample high vacuum compatibility requirement for stable SIMS analysis (10-8 to 10-9 torr). Some naturally occurring calcite has apparent utility as a reference material. For example, equigranular calcite from some zones of carbonatite intrusions (sovites) and recrystallized calcites from highly metamorphosed metallic ore deposits. Most calcite marbles, though possibly appropriate as Sr standards, show substantial inhomogeneity in Mg, Mn and Ba. Some hydrothermal “Iceland Spar” calcite may prove useful as a reference for extremely low concentrations of Mg, Sr and Ba. The best carbonatitic calcites currently in use appear homogeneous to

Doorways III: Teacher Reference Materials. On School-Related Gender-Based Violence Prevention and Response

Science.gov (United States)

US Agency for International Development, 2009

2009-01-01

The Doorways training program was designed by the U.S. Agency for International Development (USAID)-funded Safe Schools Program (Safe Schools) to enable teachers, community members and students to prevent and respond to school-related gender-based violence (SRGBV). This booklet, "Doorways III: Teacher Reference Materials on School-Related…

Compilation of elemental concentration data for NBS Biological and Environmental Standard Reference Materials

International Nuclear Information System (INIS)

Gladney, E.S.

1980-07-01

Concentration data on up to 76 elementals in 19 NBS Standard Reference Materials have been collected from 325 journal articles and technical reports. These data are summarized into mean +- one standard deviation values and compared with available data from NBS and other review articles. Data are presented on the analytical procedures employed and all raw data are presented in appendixes

Production and certification of reference materials; Producao e certificacao de materiais de referencia

Energy Technology Data Exchange (ETDEWEB)

Sarkis, Jorge Eduardo de S.; Kakazu, Mauricio H; Hespanhol, Emilio Carlos B; Martins, Elaine Arantes J [Instituto de Pesquisas Energeticas e Nucleares (IPEN), Sao Paulo, SP (Brazil)

1996-07-01

The reference materials used in analytical chemistry permit us to evaluate correctly the analytical producers as well as experimental set up. U{sub 3} O{sub 8} was produced at IPEN to be used as a secondary standard. We present the first results on U{sub 3} O{sub 8} and discuss the method, preparation, and characterization of that oxide. (author)

Determination of trace elements in standard reference materials by the ko-standardization method

International Nuclear Information System (INIS)

Smodis, B.; Jacimovic, R.; Stegnar, P.; Jovanovic, S.

1990-01-01

The k o -standardization method is suitable for routine multielement determinations by reactor neutron activation analysis (NAA). Investigation of NIST standard reference materials SRM 1571 Orchard Leaves, SRM 1572 Citrus leaves, and SRM 1573 Tomato Leaves showed the systematic error of 12 certified elements determined to be less than 8%. Thirty-four elements were determined in NIST proposed SRM 1515 Apple Leaves

Determination of Natural Levels of Radionuclides in Proposed Mushroom Reference Material (A Proficiency Test Exercise)

International Nuclear Information System (INIS)

Waheed, S.; Rahman, A.; Siddique, N.; Ahmad, S.; Zaidi, J.H.

2006-08-01

A proficiency test (PT) was organized within the framework of international Atomic Energy Agency (IAEA) project INT/1/054, entitled 'Preparation' of Reference Materials and Organization of Proficiency Test Rounds'. This exercise served to estimate the proficiency of the analytical laboratories from participating countries. This report presents the results of the proficiency test exercise on the proposed Mushroom Reference Material for the determination of natural levels of radionuclides. Laboratories from 6 different countries submitted data on the following three radionuclides: /sup 134/Cs, /sup 137/Cs, /sup 40/K. Results for /sup 134/Cs, 137/sup 137/Cs, and /sup 40/K in the mushroom reference material were reported by three or more participating laboratories and could be subjected to statistical evaluation. The original data of these raionuclides was subjected to a computer program 'Histo Vession 2.1' provided by IAEA. The four outlier tests i.e. Dixon, Grubbs, Skewness and Kurtosis were applied to the data sets. All values for these three radionuclides were accepted by the software. Consensus (overall) mean value, absolute standard deviation, relative standard deviation, standard error, median and range of values for these three radionuclides have been are obtained (at significance level 0.05). the consensus mean values and confidence intervals are given./sup 134/Cs: 4.4 Bq/kg (3.4-5.3 Bq/kg) /sup 137/Cs: 2899 Bq/kg (2740-3058 Bq/kg) /sup 40/K: 1136 Bq/kg (1046-1226 Bq/kg). (author)

Compressive strength and interfacial transition zone of sugar cane bagasse ash concrete: A comparison to the established pozzolans

Science.gov (United States)

Hussein, Asma Abd Elhameed; Shafiq, Nasir; Nuruddin, Muhd Fadhil

2015-05-01

Agricultural and industrial by-products are commonly used in concrete production as cement replacement materials (CRMs) or as admixtures to enhance both fresh and hardened properties of concrete as well as to save the environment from the negative effects caused by their disposal. Sugar Cane Bagasse Ash (SCBA) is one of the promising CRMs, it is used as a partial replacement of cement for producing concrete; properties of such concrete depend on the chemical composition, fineness, and burning temperature of SCBA. Approximately 1500 Million tons of sugarcane are annually produced over all the world which leave about 40-45% bagasse after juice crushing for sugar industry giving an average annual production of about 600 Million tons of bagasse as a waste material. This paper presents some findings on the effect of SCBA on workability, compressive strength and microstructure of interfacial zone of concrete and its performance is compared to some of the established CRMs namely Densified Silica Fume, Fly Ash and Microwave Incinerated Rice Husk Ash.

Preparation and certification of arsenate [As(V)] reference material, NMIJ CRM 7912-a.

Science.gov (United States)

Narukawa, Tomohiro; Kuroiwa, Takayoshi; Narushima, Izumi; Jimbo, Yasujiro; Suzuki, Toshihiro; Chiba, Koichi

2010-05-01

Arsenate [As(V)] solution reference material, National Metrology Institute of Japan (NMIJ) certified reference material (CRM) 7912-a, for speciation of arsenic species was developed and certified by NMIJ, the National Institute of Advanced Industrial Science and Technology. High-purity As(2)O(3) reagent powder was dissolved in 0.8 M HNO(3) solution and As(III) was oxidized to As(V) with HNO(3) to prepare 100 mg kg(-1) of As(V) candidate CRM solution. The solution was bottled in 400 bottles (50 mL each). The concentration of As(V) was determined by four independent analytical techniques-inductively coupled plasma mass spectrometry, inductively coupled plasma optical emission spectrometry, graphite furnace atomic absorption spectrometry, and liquid chromatography inductively coupled plasma mass spectrometry-according to As(V) calibration solutions, which were prepared from the arsenic standard of the Japan Calibration Service system and whose species was guaranteed to be As(V) by NMIJ. The uncertainties of all the measurements and preparation procedures were evaluated. The certified value of As(V) in the CRM is (99.53 +/- 1.67) mg kg(-1) (k = 2).

Quality assessment of organic coffee beans for the preparation of a candidate reference material

International Nuclear Information System (INIS)

Tagliaferro, F.S.; Nadai Fernandes de, E.A.; Bacchi, M.A.

2006-01-01

A random sampling was carried out in the coffee beans collected for the preparation of the organic green coffee reference material in view of assessing the homogeneity and the presence of soil as impurity. Fifteen samples were taken for the between-sample homogeneity evaluation. One of the samples was selected and 10 test portions withdrawn for the within-sample homogeneity evaluation. Br, Ca, Co, Cs, Fe, K, Na, Rb, Sc and Zn were determined by instrumental neutron activation analysis (INAA). The F-test demonstrated that the material is homogeneous for Ca, Co, Cs, K and Sc, but not homogeneous for Br, Fe, Na, Rb and Zn. Results of terrigenous elements suggested negligible soil contamination in the raw material. (author)

A study on some trace elements in Chilean seafood

Energy Technology Data Exchange (ETDEWEB)

Gras, N; Munoz, L; Thieck, M; Hurtado, S [Comision Chilena de Energia Nuclear, Santiago (Chile). Lab. of Activation Analysis

1993-03-01

Levels of essential and toxic trace elements in six marine species greatly in demand in the international market (canned pink clams, razor clams, clams, king crab, sardines, and frozen albacore tuna fish) were studied. A special laboratory adequately equipped for handling and preparing biological materials, is described. The elements As, Br, Na, Se, Hg, Cr, Fe, Zn and Rb were determined by INAA, while copper and cadmium content were determined using RNAA. Significant differences were found on comparing the contents of some toxic elements in mollusk and other samples of marine food. Various certified reference materials (CRMs) of the IAEA, NIST and NIES were analyzed for quality assurance purposes. (author) 11 refs.; 1 fig.; 1 tab.

A study on some trace elements in Chilean seafood

International Nuclear Information System (INIS)

Gras, N.; Munoz, L.; Thieck, M.; Hurtado, S.

1993-01-01

Levels of essential and toxic trace elements in six marine species greatly in demand in the international market (canned pink clams, razor clams, clams, king crab, sardines, and frozen albacore tuna fish) were studied. A special laboratory adequately equipped for handling and preparing biological materials, is described. The elements As, Br, Na, Se, Hg, Cr, Fe, Zn and Rb were determined by INAA, while copper and cadmium content were determined using RNAA. Significant differences were found on comparing the contents of some toxic elements in mollusk and other samples of marine food. Various certified reference materials (CRMs) of the IAEA, NIST and NIES were analyzed for quality assurance purposes. (author) 11 refs.; 1 fig.; 1 tab

Closed vessel miniaturized microwave assisted chelating extraction for determination of trace metals in plant materials

Science.gov (United States)

Czarnecki, Sezin; Duering, Rolf-Alexander

2013-04-01

In recent years, the use of closed vessel microwave assisted extraction (MAE) for plant samples has shown increasing research interest which will probably substitute conventional procedures in the future due to their general disadvantages including consumption of time and solvents. The objective of this study was to demonstrate an innovative miniaturized closed vessel microwave assisted extraction (µMAE) method under the use of EDTA (µMAE-EDTA) to determine metal contents (Cd, Co, Cu, Mn, Ni, Pb, Zn) in plant samples (Lolio-Cynosuretum) by inductively coupled plasma-optical emission spectrometry (ICP-OES). Validation of the method was done by comparison of the results with another miniaturized closed vessel microwave HNO3 method (µMAE-H) and with two other macro scale MAE procedures (MAE-H and MAE-EDTA) which were applied by using a mixture of nitric acid (HNO3) and hydrogen peroxide (H2O2) (MAE-H) and EDTA (MAE-EDTA), respectively. The already established MAE-H method is taken into consideration as a reference validation MAE method for plant material. A conventional plant extraction (CE) method, based on dry ashing and dissolving of the plant material in HNO3, was used as a confidence comparative method. Certified plant reference materials (CRMs) were used for comparison of recovery rates from different extraction protocols. This allowed the validation of the applicability of the µMAE-EDTA procedure. For 36 real plant samples with triplicates each, µMAE-EDTA showed the same extraction yields as the MAE-H in the determination of Cd, Co, Cu, Mn, Ni, Pb, and Zn contents in plant samples. Analytical parameters in µMAE-EDTA should be further investigated and adapted for other metals of interest. By the reduction and elimination of the use of hazardous chemicals in environmental analysis and thus allowing a better understanding of metal distribution and accumulation process in plants and also the metal transfer from soil to plants and into the food chain, µ

Neutron activation analysis of trace elements in a marine sediment reference material

International Nuclear Information System (INIS)

Esquivel, D.; Eguren, L.; Montoya, E.

1993-01-01

As part of the second intercomparison run of ARCAL-IV, it was analyzed the marine sediment, reference materials PACS-NR CC1 by INAA, in the RP-10 Reactor with a thermal flux of 7,8 x 10 13 n/cm 2 s. The results obtained (± 1σ,n=4) were: Co: 17,2±0,8 ppm; Cr:97,8±0,6 ppm; Fe: 46,0± 0,7 ppm; Na: 31,0±1,09/kg; Sb: 175±5 ppm; in good agreement with the certified values. The results in ppm (±18,n=4), for non certified elements were:Ba: 730±58; Ce: 25±3; Cs: 3,8±0,8; Eu: 1,00±0,03; Hf: 3,30±0,07; Lu:0,25±0,04; Rb: 44,0±0,9; Sc: 14,40±0,04; Sm: 3,4±0,5; Ta: 0,60±0,03; Tb: 0,5±0,05; Th: 3,80±0,02; U: 2,6±0,4; which are in good agreement with other three Latin American and one European INAA Laboratories. It was used the comparative method with AGV-1, GSP-1 and G-2 , USGS reference materials, as standards. (authors). 7 refs., 4 tabs

Introducing LIR (Lithotheque Ireland, a reference collection of flaked stone tool raw materials from Ireland

Directory of Open Access Journals (Sweden)

Killian Driscoll

2016-09-01

Full Text Available The LIR (Lithotheque Ireland reference collection of flaked stone tool raw materials from Ireland began in 2013, and is based on the geological prospection from two projects. The first (2013-2015 focused attention primarily on Carboniferous cherts from the northwest of Ireland, collecting 405 samples. The second (2015-2017 is currently collecting samples of the Cretaceous flint primarily from in situ contexts in the northeast of Ireland, but also includes beach surveys of Cretaceous flint from around the island; the first phase of geological prospection in Autumn 2015 collected 239 samples, with the geological prospection continuing in 2016. Therefore, to date the collection contains over 600 hand samples of chert and flint, along with a small number of other materials (siliceous limestone, tuff, mudstone. The physical reference collection is housed at the UCD School of Archaeology, University College Dublin and contains the geological hand samples along with the various thin sections of the samples that are used for petrographic analysis. The physical collection is complemented by an online database that is to be used alongside the physical collection, or can be used as a stand-alone resource. This paper provides an overview of the database’s metadata and the processes of data entry and editing, to serve as a reference point for the database and the fieldwork undertaken to date, and to serve as a template for other researchers undertaking similar work on lithic reference collections.

Challenges in the size analysis of a silica nanoparticle mixture as candidate certified reference material

International Nuclear Information System (INIS)

Kestens, Vikram; Roebben, Gert; Herrmann, Jan; Jämting, Åsa; Coleman, Victoria; Minelli, Caterina; Clifford, Charles; Temmerman, Pieter-Jan De; Mast, Jan; Junjie, Liu; Babick, Frank; Cölfen, Helmut; Emons, Hendrik

2016-01-01

A new certified reference material for quality control of nanoparticle size analysis methods has been developed and produced by the Institute for Reference Materials and Measurements of the European Commission’s Joint Research Centre. The material, ERM-FD102, consists of an aqueous suspension of a mixture of silica nanoparticle populations of distinct particle size and origin. The characterisation relied on an interlaboratory comparison study in which 30 laboratories of demonstrated competence participated with a variety of techniques for particle size analysis. After scrutinising the received datasets, certified and indicative values for different method-defined equivalent diameters that are specific for dynamic light scattering (DLS), centrifugal liquid sedimentation (CLS), scanning and transmission electron microscopy (SEM and TEM), atomic force microscopy (AFM), particle tracking analysis (PTA) and asymmetrical-flow field-flow fractionation (AF4) were assigned. The value assignment was a particular challenge because metrological concepts were not always interpreted uniformly across all participating laboratories. This paper presents the main elements and results of the ERM-FD102 characterisation study and discusses in particular the key issues of measurand definition and the estimation of measurement uncertainty.

Challenges in the size analysis of a silica nanoparticle mixture as candidate certified reference material

Energy Technology Data Exchange (ETDEWEB)

Kestens, Vikram, E-mail: vikram.kestens@ec.europa.eu; Roebben, Gert [Joint Research Centre (JRC), European Commission, Institute for Reference Materials and Measurements (IRMM) (Belgium); Herrmann, Jan; Jämting, Åsa; Coleman, Victoria [National Measurement Institute Australia, Nanometrology Section (Australia); Minelli, Caterina; Clifford, Charles [National Physical Laboratory, Analytical Science Division (United Kingdom); Temmerman, Pieter-Jan De; Mast, Jan [Service Electron Microscopy, Veterinary and Agrochemical Research Centre (CODA-CERVA) (Belgium); Junjie, Liu [National Institute of Metrology, Division of Nanoscale Measurement and Advanced Materials (China); Babick, Frank [Technische Universität Dresden, Institut für Verfahrens- und Umwelttechnik (Germany); Cölfen, Helmut [University of Konstanz, Physical Chemistry, Department of Chemistry (Germany); Emons, Hendrik [Joint Research Centre (JRC), European Commission, Institute for Reference Materials and Measurements (IRMM) (Belgium)

2016-06-15

A new certified reference material for quality control of nanoparticle size analysis methods has been developed and produced by the Institute for Reference Materials and Measurements of the European Commission’s Joint Research Centre. The material, ERM-FD102, consists of an aqueous suspension of a mixture of silica nanoparticle populations of distinct particle size and origin. The characterisation relied on an interlaboratory comparison study in which 30 laboratories of demonstrated competence participated with a variety of techniques for particle size analysis. After scrutinising the received datasets, certified and indicative values for different method-defined equivalent diameters that are specific for dynamic light scattering (DLS), centrifugal liquid sedimentation (CLS), scanning and transmission electron microscopy (SEM and TEM), atomic force microscopy (AFM), particle tracking analysis (PTA) and asymmetrical-flow field-flow fractionation (AF4) were assigned. The value assignment was a particular challenge because metrological concepts were not always interpreted uniformly across all participating laboratories. This paper presents the main elements and results of the ERM-FD102 characterisation study and discusses in particular the key issues of measurand definition and the estimation of measurement uncertainty.

Comprehensive inter-laboratory calibration of reference materials for δ18O versus VSMOW using various on-line high-temperature conversion techniques

Science.gov (United States)

Brand, Willi A.; Coplen, Tyler B.; Aerts-Bijma, Anita T.; Bohlke, John Karl; Gehre, Matthias; Geilmann, Heike; Groning, Manfred; Jansen, Henk G.; Meijer, Harro A. J.; Mroczkowski, Stanley J.; Qi, Haiping; Soergel, Karin; Stuart-Williams, Hilary; Weise, Stephan M.; Werner, Roland A.

2009-01-01

Internationally distributed organic and inorganic oxygen isotopic reference materials have been calibrated by six laboratories carrying out more than 5300 measurements using a variety of high-temperature conversion techniques (HTC) in an evaluation sponsored by the International Union of Pure and Applied Chemistry (IUPAC). To aid in the calibration of these reference materials, which span more than 125‰, an artificially enriched reference water (δ18O of +78.91‰) and two barium sulfates (one depleted and one enriched in 18O) were prepared and calibrated relative to VSMOW2 and SLAP reference waters. These materials were used to calibrate the other isotopic reference materials in this study, which yielded:Reference materialδ18O and estimated combined uncertainty IAEA-602 benzoic acid+71.28 ± 0.36‰USGS35 sodium nitrate+56.81 ± 0.31‰IAEA-NO-3 potassium nitrate+25.32 ± 0.29‰IAEA-601 benzoic acid+23.14 ± 0.19‰IAEA-SO-5 barium sulfate+12.13 ± 0.33‰NBS 127 barium sulfate+8.59 ± 0.26‰VSMOW2 water0‰IAEA-600 caffeine−3.48 ± 0.53‰IAEA-SO-6 barium sulfate−11.35 ± 0.31‰USGS34 potassium nitrate−27.78 ± 0.37‰SLAP water−55.5‰The seemingly large estimated combined uncertainties arise from differences in instrumentation and methodology and difficulty in accounting for all measurement bias. They are composed of the 3-fold standard errors directly calculated from the measurements and provision for systematic errors discussed in this paper. A primary conclusion of this study is that nitrate samples analyzed for δ18O should be analyzed with internationally distributed isotopic nitrates, and likewise for sulfates and organics. Authors reporting relative differences of oxygen-isotope ratios (δ18O) of nitrates, sulfates, or organic material should explicitly state in their reports the δ18O values of two or more internationally distributed nitrates (USGS34, IAEA-NO-3, and USGS35), sulfates (IAEA-SO-5, IAEA

Reference material manufacture and certification for the AVNG

Energy Technology Data Exchange (ETDEWEB)

Hauck, Danielle K [Los Alamos National Laboratory; Thron, Jonathan [Los Alamos National Laboratory; MacArthur, Duncan W. [Los Alamos National Laboratory; Livke, Alexander [RFNC - VNIIEF; Bulatov, M [RFNC-VNIIEF; Kondratov, Sergey [RFNC-VNIIEF; Leplyavkina, M [RFNC-VNIIEF; Razinkov, Sergey [RFNC-VNIIEF; Sivachev, D [RFNC-VNIIEF; Tsybryaev, S [RFNC-VNIIEF; V' yushin, A [RFNC-VNIIEF

2010-07-09

Testing and demonstration of any radiation measurement system requires the use of appropriate radioactive sources. An attribute measurement system (A VNG) was developed and fabricated at the Russian Federal Nuclear Center, VNIIEF, Russia, under contract with LANL, USA. The A VNG detects neutron and gamma radiation signatures and compares the data analysis results with the specified threshold values for three unclassified attributes; plutonium is present or absent, plutonium mass is greater than or less than the specified threshold value and plutonium isotopic ratio ²⁴⁰Pu to ²³⁹Pu) is greater than or less then the threshold value. A set of reference materials (RMs) was specially manufactured for the A VNG with masses and isotopic ratios above and below the selected thresholds. The set of RMs was certified in compliance with the Russian metrological requirements. The RMs were used to debug and test the A VNG and to demonstrate the A VNG operation to an American delegation in June 2009. In this presentation, we will describe the various steps in the manufacture and certification of these RM sources.

Reference material manufacture and certification for the AVNG

Energy Technology Data Exchange (ETDEWEB)

Hauck, Danielle K [Los Alamos National Laboratory; Mac Arthur, Duncan [Los Alamos National Laboratory; Thron, Jonathan L [Los Alamos National Laboratory; Livke, Alexander [VNIIEF; Kondratov, Sergey [VNIIEF; Razinkov, Sergey [VNIIEF

2010-01-01

Testing and demonstration of any radiation measurement system requires the use of appropriate radioactive sources. The AVNG implementation that we describe is an attribute measurement system built by RFNC - VNIIEF in Sarov, Russia. The AVNG detects neutron and gamma radiation signatures and displays the three unclassified attributes of 'plutonium presence,' 'plutonium mass > 2 kg,' and 'plutonium isotopic ratio ({sup 240}Pu to {sup 239}Pu) < 0.1.' The AVNG was tested using a number of reference material (RM) sources with masses and isotopic ratios above and below these thresholds. The AVNG was demonstrated in June 2009 using several of these sources in addition to detector calibration sources. Since the AVNG was designed to measure multi-kg plutonium sources, the RM was manufactured specifically for use with this system. In addition, the RM was used to test the thresholds in the AVNG, so the size and composition of each RM was certified prior to use. In this presentation, we will describe the various steps in the manufacture and certification of these RM sources.